CN113248244B - 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 PDFInfo
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- CN113248244B CN113248244B CN202110550711.6A CN202110550711A CN113248244B CN 113248244 B CN113248244 B CN 113248244B CN 202110550711 A CN202110550711 A CN 202110550711A CN 113248244 B CN113248244 B CN 113248244B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
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- 238000002156 mixing Methods 0.000 claims abstract description 29
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- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 15
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- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 2
- 239000005995 Aluminium silicate Substances 0.000 claims description 2
- 235000012211 aluminium silicate Nutrition 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- ZZNQQQWFKKTOSD-UHFFFAOYSA-N diethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OCC)(OCC)C1=CC=CC=C1 ZZNQQQWFKKTOSD-UHFFFAOYSA-N 0.000 claims description 2
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 claims description 2
- AHUXYBVKTIBBJW-UHFFFAOYSA-N dimethoxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](OC)(OC)C1=CC=CC=C1 AHUXYBVKTIBBJW-UHFFFAOYSA-N 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims 7
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- 229910010293 ceramic material Inorganic materials 0.000 abstract description 15
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 238000013001 point bending Methods 0.000 description 4
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- 239000000377 silicon dioxide Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
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- 230000015556 catabolic process Effects 0.000 description 2
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- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
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- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
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- 238000001878 scanning electron micrograph Methods 0.000 description 1
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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
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 mainly of ionic structure and include mica, ceramics, glass and the like. The mixed insulating material is formed by mixing 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 performance, good insulating performance and mechanical strength, electric arc resistance, aging resistance, mould pressing or pouring forming 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 becoming more difficult to cope with complicated working environments, and failures have also developedThere are not a few. 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, al 2 O 3 The sintering temperature of the ceramic is 1650-1950 ℃ according to different components, and the hot-pressed and sintered Si 3 N 4 The hot pressing temperature is generally 1600-1800 ℃, when the AlN ceramic is sintered under no pressure, the sintering temperature is about 1800 ℃, and the hot pressing sintering is carried out at a high temperature of 1800-2000 ℃. Therefore, the sintering temperature of the common ceramic is generally higher than the melting point of the copper wire (1083.4 ℃), and the application in the fields of electrical equipment and the like has great limitation.
Guo Jianhua et al invented a low temperature ceramizable silicone rubber and its preparation method (CN 107163585A), and prepared a composite silicone rubber material, which is used in the flame retardant and fire resistant fields of wire and cable. 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 silicone rubber material, sintering and ceramization are not needed, and only a ceramic body but not the composite silicone 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 Guo Jianhua 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 in the proportions of the 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 low-temperature ceramic silicon rubber, and the low-temperature ceramic silicon rubber is a ceramic insulating material, is a ceramic product in a final form, has excellent properties of a ceramic material and is substantially different from a composite silicon rubber material. The obtained ceramic insulating material has a density of 2.15-2.18 g/cm -3 The 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 0.6mm 2 ·s -1 -0.8mm 2 ·s -1 Has a thermal conductivity in the range of 1.2 W.m -1 ·K -1 -1.7W·m -1 ·K -1 The volume resistivity is (3.101-3.111) × 10 12 Ω · m, relative dielectric constant of 8.09-8.12, tan delta value of (9.30-9.38) × 10 -4 The power frequency breakdown field intensity is (21.01-21.31) kV · mm -1 The 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. Guo Jianhua et al invented 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. For the present hairSpecifically, according to the method, 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, the silicon dioxide participates in the subsequent ceramic forming reaction, and finally the ceramic insulating material meeting the requirements of the complex insulating structure is obtained. Meanwhile, the section of the ceramic insulating material is flat and compact, 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 silicone rubber of Guo Jianhua and the like is only 3.1-5.9MPa, the flatness and the compactness of the ceramic layer are limited, the research on the insulating property and the heat conducting property of the ceramic layer is lacked, the use efficiency requirement of the ceramic insulating material is not met, and the application requirements of severe working conditions such as high temperature, corrosion, radiation and the like cannot be met. 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.
Furthermore, 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 one or more other sulfurizing 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 fumed silica, and 2 percent of hydroxyl silicone oil and 2,4-dichlorobenzoyl peroxide in total.
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 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, 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 silicon rubber, then fumed silica is slowly added in batches for multiple times, after the mixture is uniform, wollastonite and low-melting-point glass powder are added, finally a vulcanizing agent is added, and after the mixture is uniform, the mixture is mixed and mixed.
Further, in the vulcanization treatment, the mixture is subjected to primary vulcanization at 120 ℃ for 5-20min, and then subjected to secondary vulcanization at 150 ℃ for 3-5h.
Further, during sintering, aluminum oxide powder is used for burning, the heating rate is 1 ℃/min, and the heat preservation time is 1-2h.
Compared with the preparation process of Guo Jianhua and the like, the preparation process of the invention is similar to the preparation process of the invention due to the fact that 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 the silicon rubber composite material can be obtained after sintering. Therefore, the preparation method of the patent should obviously 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 Guo Jianhua and the like, the ceramic insulating material disclosed by the invention 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 ceramic formation 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 sintering is carried out, the ceramic body finished product obtained after sintering into ceramic has excellent properties of ceramic material, corrosion resistance, high temperature resistance, radiation resistance and heat conductivity, and meanwhile, the ceramic forming temperature of the ceramic material is reduced, so that a compact ceramic body is prepared at 1000 ℃, the ceramic 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 porcelain 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, respectively weighing porcelain forming filler, low-melting-point fluxing agent, fumed silica, functional additive and methyl vinyl silicone rubber in proportion for later use;
s2, because the methyl vinyl silicone rubber is soft and fluid at normal temperature, 10-20% (mass fraction) 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 rubber material needs to be added in batches, multiple times, in small amount 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 a vulcanizing agent 2,4-dichlorobenzoyl peroxide, wherein the total amount of the vulcanizing agent and the structural control agent is 1-3%, and the preferred mixing amount is 2%, and taking out and weighing after all the raw materials are uniformly mixed to obtain a mixture;
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, and then carrying out secondary vulcanization by using an electric heating blast box at the secondary vulcanization temperature of 150 ℃ for 4h to obtain a precursor, cutting and molding the precursor, wherein the precursor can be cut into a required shape by using a special cutter during cutting and 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 process, wherein Al is adopted 2 O 3 Burying 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 -1 Namely, 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 addition of the fumed silica is finished, 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 4 hours, so as to obtain a vulcanized precursor;
s3, cutting the vulcanized precursor into a small 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 process, wherein Al is adopted 2 O 3 Burying and burning the powder; in the sintering process, the temperature gradient is set to be 50 ℃ from the normal temperature, and the heating rate is 1 ℃ min -1 And 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 4 hours, so as to obtain a vulcanized precursor;
s3, cutting the vulcanized precursor into a square 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 adopted 2 O 3 Burying 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 -1 And 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 addition of the fumed silica is finished, 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 4 hours, 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 adopted 2 O 3 Burying 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 -1 And 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 4 hours, 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 by using Al 2 O 3 Burying 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 -1 And 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
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 -3 The 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 0.6mm 2 ·s -1 -0.8mm 2 ·s -1 Has a thermal conductivity in the range of 1.2 W.m -1 ·K -1 -1.7W·m -1 ·K -1 Volume resistivity of (3.101-3.111) × 10 12 Omega. M, a relative dielectric constant of 8.09 to 8.12, tan delta of (9.30 to 9.38) × 10 -4 The power frequency breakdown field intensity is (21.01-21.31) kV · mm -1 The 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 intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (8)
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%; the porcelain forming filler is one or more of wollastonite, mica, diatomite, kaolin and fiber fillers; the preparation method of the ceramic insulating material comprises 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, 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.
2. 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.
3. 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.
4. The low temperature ceramified ceramic insulation suitable for use in complex insulation structures as defined in 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.
5. 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 fumed silica, and 2 percent of hydroxyl silicone oil and 2,4-dichlorobenzoyl peroxide in total.
6. The low-temperature ceramic insulating material suitable for complex insulating structures as claimed in claim 1, wherein in S1, the structure-controlling agent is added to the silicone rubber, then the fumed silica is slowly added in batches in multiple times, after uniform mixing, the wollastonite and the low-melting-point glass powder are added, and finally the vulcanizing agent is added, and after uniform mixing, mixing is carried out.
7. The low temperature ceramicized ceramic insulating material for complex insulating structure as claimed in claim 6, wherein the mixture is first vulcanized at 120 ℃ for 5-20min and then second vulcanized at 150 ℃ for 3-5h in vulcanization treatment.
8. The low temperature ceramic insulating material for complex insulating structures of claim 7, wherein during sintering, aluminum oxide powder is used for burying and burning, the heating rate is 1 ℃/min, and the holding time is 1-2h.
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