CN102254647B - Composite insulating material and preparation method thereof - Google Patents
Composite insulating material and preparation method thereof Download PDFInfo
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- CN102254647B CN102254647B CN 201110122892 CN201110122892A CN102254647B CN 102254647 B CN102254647 B CN 102254647B CN 201110122892 CN201110122892 CN 201110122892 CN 201110122892 A CN201110122892 A CN 201110122892A CN 102254647 B CN102254647 B CN 102254647B
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Abstract
The invention provides a composite insulating material, a polymer insulating substrate material and a nanometer composite coating; the nanometer composite coating comprises an organic silicon resin, nanometer titanium dioxide and fluorophlogopite; the nanometer composite coating is coated on the surface of the polymer insulating substrate material. In the nanometer composite coating, the content of the organic silicon resin is 40-75 wt%, the content of the nanometer titanium dioxide is 20-40 wt%, and the content of the fluorophlogopite is 5-20 wt%; preferably, the content of the organic silicon resin is 50-70 wt%, the content of the nanometer titanium dioxide is 25-40 wt%, and the content of the fluorophlogopite is 8-13 wt%. The prepared composite insulating material has the advantages of low dielectric constant, high vacuum flashover voltage, low-surface secondary electronic emission coefficient and good weather resistance. The invention further provides a preparation method of the composite insulating material.
Description
Technical field
The present invention relates to a kind of composite insulating material, be specifically related to a kind of nylon insulator composite with good vacuum insulation performance.The invention still further relates to above-mentioned composite manufacture technique.
Background technology
The edge flashing phenomenon is a major issue of vacuum electric equipment, insulation flashover makes the voltage endurance capability of insulating material in the vacuum be significantly less than the vacuum gap of same distance, and the insulating material vacuum flashover voltage that whole high pressure vacuum electric equipment adopts becomes the bottleneck of the ceiling voltage that the whole equipment of restriction can bear.Along with day by day highlighting that High pulse power technology acts in national economy and national defense construction, many large-scale tip device, such as burst pulse high-power microwave source, high current particle beam accelerator, emerging high power pulsed laser etc., these pulse power devices are to high power more, more high power capacity, the future development of miniaturization more, and this has higher requirement to vacuum insulation edge flashing intensity.Therefore, significant to the coating material research with good vacuum insulation flashover property.
Insulator is mounted between the conductor of different potentials or between conductor and the earth potential member, can withstand voltage and the device of mechanical stress effect.Its effect is that the electric conductor that will be in different potentials mechanically interconnects, mutually insulated on electric.The electric property of insulator usually with between two electrodes along the discharge voltage of insulator exterior, namely flashover voltage is weighed.Generally, the energized conductor overwhelming majority that insulator and it fix is in air, if the voltage to earth of raising energized conductor, will be on the interface of insulator and air Discharge Phenomena, this discharge is called creeping discharge.Creeping discharge develops into perfoliate punch-through and is called flashover.Under high electric field action; disruptive discharge phenomenon along the solid insulation surface usually can occur in vacuum, gas or liquid medium; it is dielectric surface flashover; and the voltage that flashover occurs is wherein especially serious with the flashover phenomenon in the vacuum often far below the puncture voltage of solid and atmosphere medium itself.
The reason of insulator generation flashover in the vacuum, not to puncture because the body of insulator has occured, because the bulk breakdown voltage of dielectric usually above same apart from the vacuum gap puncture voltage, in fact, the basic reason that voltage endurance capability reduces behind the lead-in insulator is because at insulator surface edge flashing has occured, and namely along vacuum one insulator interface the penetrability electric breakdown phenomena has occured.
The existence of vacuum edge flashing phenomenon has restricted the electric property of many electron tubes, has affected especially the normal operation of relevant tip device, even has caused huge loss.Because the edge flashing voltage of the solid insulating material bulk breakdown voltage under the equal insulation distance, in the pulse power device because the insulation breakdown that edge flashing causes is modal.It is reported, accelerator in the klystron at Stanford Univ USA linear accelerator center, the Japanese high-energy physics National Laboratory and the accelerator of the CEBAF of USDOE all once occured because the problem that insulator edge flashing phenomenon causes in the vacuum, large-scale tip device is damaged, huge economic loss (A.E.Vlieks etc. have been caused, IEEE Transactions on Electrical Insulation, 24 (1989): 1023-1028).The surface characteristic of solid insulating material greatly affects its vacuum edge flashing characteristic, and this phenomenon is greatly restricting the overall performance of vacuum insulation systems for a long time, has limited the development process of high-voltage electric vacuum equipment.Therefore seek a kind of coating process, to improve the flashover voltage of the insulator in the vacuum, for the normal operation of guaranteeing large-scale tip device very important meaning is arranged.
In the prior art, comprise that epoxy resin casting solidification method prepares insulator (referring to CN101221832) and the standby organosilicon insulating material (referring to CN1297232) of room temperature silicone sulfuration legal system.Epoxy resin casting solidification method is to adopt epoxy-resin systems and other uniform filling to mix, and vacuum treatment is molded into bubble-free raw material in all kinds of insulator moulds, and vacuum solidification is prepared into the composite insulating material with the aging ability of anti-branch.The A component that room temperature silicone sulfuration method is formed by organopolysiloxane, reinforced filling, antistructurizing agent etc. and mix the organic silicon insulation material that room temperature vulcanization is made by the B component that crosslinking agent forms.But there is poor heat resistance in epoxy resin as the insulator cast material, the deficiency that intensity is relatively low, and the crosslinking agent ordinary-temp sulfurizing process need to mix two kinds of components and sulfuration in preparation process, technique is relatively complicated.And above-mentioned two kinds of inventions all are not suitable for the transformation of existing insulator.
Nylon 1010 is nylon 1010, is a kind of widely used insulator base material, and its long-chain molecule structure and crystallization make it have good Physical and mechanical properties.Yet because the existence of acid amides polar group, the water absorption rate of nylon 1010 insulator is high, and dielectric stability is relatively poor, modulus and intensity are high not enough, and as the insulator manufactured materials, its application has been subject to certain restriction, need to carry out material modification, to improve its vacuum insulation performance.
Summary of the invention
The object of the present invention is to provide a kind of composite insulating material that is coated with nano-composite coating, have higher vacuum flashover voltage, and have low surface second electron emission coefficiency, what good weatherability of low-k.The present invention also provides the preparation method of above-mentioned nano-composite coating.
The invention provides a kind of composite insulating material, macromolecule insulating body material and nano-composite coating, described nano-composite coating comprises organic siliconresin, nano titanium oxide and fluorophologopite, and described nano-composite coating is coated in the surface of macromolecule insulating body material.
In the above-mentioned composite insulating material, the content of described organic siliconresin is 40～75wt%, and the content of nano titanium oxide is 20～40wt%, and the content of fluorophologopite is 5～20wt%.Preferably, the content of organic siliconresin is 50～70wt%, and the content of nano titanium oxide is 25～40wt%, and the content of fluorophologopite is 8～13wt%.
In the above-mentioned composite insulating material, described organic siliconresin is preferably silicone glass resin.Silicone glass resin is take methyl triethoxysilane as primary raw material, the methyl silicon resin prepolymer that makes through hydrolytic condensation; Under the normal temperature, glass resin is colourless liquid to little yellow transparent.Described nano titanium oxide is Detitanium-ore-type, and outward appearance is white powder, average grain diameter 30～70nm.Be white powder under the fluorophologopite normal temperature, be phyllosilicate, the molecular formula of single-chip is KMg
3(AlSi
3O
10) F
2
In the above-mentioned composite insulating material, described macromolecule insulating body material is known, such as nylon, polyester, epoxy resin etc.The preferred nylon insulator composite of above-mentioned composite insulating material, described nylon insulator material comprises nylon 1010, nylon 66 (polyhexamethylene adipamide) and nylon 6 (polycaprolactam) etc., preferred nylon 1010 insulator.White or the little yellow appearance of crystallization shape translucent, surface-brightening that described nylon 1010 has.
In the preferred embodiment of described composite insulating material, described composite insulating material is composite nylon 1010 insulators, comprise nylon 1010 insulator matrix and nano-composite coating, described nano-composite coating comprises organic siliconresin, nano titanium oxide and fluorophologopite, and described nano-composite coating is coated in the surface of nylon insulator matrix.
In above-mentioned composite nylon 1010 insulators, the content of described organic siliconresin is 40～75wt%, and the content of nano titanium oxide is 20～40wt%, and the content of fluorophologopite is 5～20wt%.Preferably, the content of organic siliconresin is 50～70wt%, and the content of nano titanium oxide is 25～40wt%, and the content of fluorophologopite is 8～13wt%.
The present invention also provides a kind of technique for preparing above-mentioned composite insulating material, comprising:
A) utilize solvent-ultrasonic wave dispersion method to prepare nano-composite coating: first nano titanium oxide and fluorophologopite dried bean noodles is dry, mixing, in anhydrous solvent, stir, carry out ultrasonic wave and process; And then the adding organic siliconresin, stir and carry out ultrasonic wave and process;
B) nano-composite coating of above-mentioned preparation is coated in the surface of macromolecule insulating body material, and solidifies.
Among the above-mentioned preparation technology, solvent for use is common solvent, such as water, acetone, benzene, toluene, ethanol; Preferred alcohol.
In above-mentioned preparation method's the preferred embodiment, comprising:
A) utilize solvent-ultrasonic wave dispersion method to prepare nano-composite coating: with nano-titanium oxide, fluorophologopite powder through dewatered drying, then mix according to certain ratio, join in a certain amount of absolute ethyl alcohol, the amount of absolute ethyl alcohol gets final product mixed-powder all can be immersed; In anhydrous dry environment, fully stir, with ultrasonic wave mixed system is carried out ultrasonic wave afterwards and process, powder fully is distributed in the alcohol solvent, and remove the gas of nano-powder absorption; Subsequently dispersion is staticly settled, after the abundant layering of solution system, pour out the absolute ethyl alcohol on solution upper strata, again silicone glass resin is poured in the dispersion, and stirring fully mixes it, process with ultrasonic wave subsequently, nano particle is evenly spread in the glass resin, make nano titanium oxide-fluorophologopite-silicone glass resin composite coating;
B) nano-composite coating with above-mentioned preparation is coated in the nylon insulator surface: the nylon insulator successively cleans in ultrasonic wave with deionized water, absolute ethyl alcohol, remove surface blot and greasy dirt, put at last the baking oven dewatered drying, the nano-composite coating that has prepared is coated to insulator surface with the method for brushing; After air-dry, put into vacuum drying chamber, reducing pressure heats up solidifies, and finally makes the nylon insulator with Nanosurface composite coating.
Among the above-mentioned preparation technology, the preferred nylon 1010 insulator of described nylon insulator; Preferred 60～90 ℃ of the temperature of described curing.Curing temperature is excessively low, and curing rate is slow; Curing temperature is too high, and the solvent boiling can make goods produce bubble.The time of described curing preferably surpasses 3h.
Prepare surface recombination type insulating material by above-mentioned technique, macromolecule insulating body material is after its surface coats one deck organic siliconresin, and its dielectric constant descends.Such as the dielectric constant of pure nylon 1010 about 13, and the nylon 1010 that composite coating applies, dielectric constant has dropped to about 6, less than the dielectric constant of general insulating material.Theoretical according to the field strength distribution at electrode-insulator-vacuum three binding site places, avoided the rapid increase of electric field at three binding site places, so the decline of dielectric constant can reduce and significantly improves its insulation property under vacuum condition.Composite coating has also improved the pure resistance part of its high-frequency resistance when reducing the dielectric constant of material, this impedance that mainly is the high-insulativity of organic siliconresin and fluorophologopite causes significantly improves.Simultaneously because the continuous phase of coating is silicone glass resin, main component is methyl triethoxysilane, compare with common organic resin, organic siliconresin is because its organic group is few, more good hydrophobicity, thermal endurance are arranged, and electrical insulation capability, be coated on the surface of macromolecule insulating body material, can improve its ageing resistace.
The test of vacuum flashover voltage is what to carry out in the nanosecond pulse vacuum insulation flashover experimental provision of building, and whole system mainly is comprised of several parts such as nanosecond pulse source, vacuum system, measuring system and grounding systems.Nanosecond pulse source is by Marx generator (maximum output voltage 300kV; Pulse rise time: 20～30ns; Pulse duration: 100ns) to the Pulse modulator charging, by gas-filled switching tube load discharge is obtained the nanosecond square-wave pulse (rise time: 10ns again; Pulse duration: 30ns).The no-load voltage waveform rising edge is about 10ns.Be applied to discharge voltage on the test product much larger than test product flashover voltage value, the flashover process occurs in rising edge of a pulse, so power taking corrugating peak value is test product flashover voltage value, and each experimental point flashover voltage value is the mean value of each time flashover voltage peak value.Vacuum flashover voltage test result proves that the flashover voltage of material improves.This is owing in the surface recombination type insulating material that obtains, have the combination property that acts synergistically between component and produce based on nano composite material, keeps the basis of each component material characteristics.When the vacuum nanosecond pulse discharge, the surface is owing to exist organosilicon and the mica of a large amount of high-insulativities, so that the secondary electron yield on surface reduces greatly, even the surface is because the desorb of gas, produce ionic charge, also because the existence of titanium dioxide, and it is led away fast, avoid forming the accumulation of electric charge, thereby improved the flashover voltage of material.Prepare composite insulating material by above-mentioned technique, nano-composite coating is coated in the surface of the macromolecule matrix material of certain insulating property (properties), final and basis material forms good composite insulating material.Be conducive to the lifting of the insulation property of insulating material, the useful life of prolongation insulating material by above-mentioned technique, and this technique have the characteristics simple, widely applicable, that cost is low.
Description of drawings
Accompanying drawing is used to provide a further understanding of the present invention, and consists of the part of specification, is used for together with embodiments of the present invention explaining the present invention, but does not consist of any restriction to embodiment of the present invention.Identical member illustrates with identical Reference numeral in the accompanying drawings, wherein:
Fig. 1 has shown the discharge test system diagram according to nylon insulator of the present invention;
Fig. 2 has shown the preparation technology's flow chart according to composite nylon insulator of the present invention;
Fig. 3 has shown according to each component schematic diagram of nano-composite coating of the present invention;
Fig. 4 has shown the test schematic diagram according to composite nylon insulator of the present invention.
Embodiment
The below engages accompanying drawing the preferred embodiments of the present invention is described, and should be appreciated that preferred embodiment described herein only is used for description and interpretation the present invention, is not limited to the present invention.
Fig. 1 shows the discharge test system diagram according to nylon insulator of the present invention.The test of vacuum flashover voltage is carried out in the nanosecond pulse vacuum insulation flashover experimental provision of building, and whole system mainly is comprised of several parts such as nanosecond pulse source, vacuum system, measuring system and grounding systems.Nylon insulator 3 to be tested is placed between plate electrode 1 and the earth terminal 2.
Fig. 2 shows the preparation technology's flow process according to nylon insulator of the present invention, and raw material is mixed according to certain proportioning, prepares nano-composite coating material, is coated in existing nylon insulator surface.Concrete preparation technology is with reference to following embodiment.
Fig. 3 has shown that each component is according to each component schematic diagram of nano-composite coating of the present invention: nano titanium oxide (Detitanium-ore-type), silicone glass resin (methyl triethoxysilane content is 50%), fluorophologopite powder.
In specific embodiments of the invention, nano titanium oxide (Detitanium-ore-type), the HTTi type nano-titanium oxide of sea, employing Nanjing Turner rice manufacture of materials, average grain diameter 30～70nm.The MS-1-50 type glass resin that silicone glass resin adopts Zhong Hao Chenguang Research Institute of Chemical Industry to produce is take methyl triethoxysilane as primary raw material, the methyl silicon resin prepolymer that makes through hydrolytic condensation.Glass resin is colourless liquid to little yellow transparent, has quick-setting at low temperatures characteristics.The fluorophologopite powder adopts the sky, Changchun to become the product of fluorophologopite Co., Ltd.
Embodiment 1:
At first with required nano titanium oxide (Detitanium-ore-type), fluorophologopite carries out drying and dewatering to be processed, 110 ℃ of lower processing 5 hours, then join in an amount of absolute ethyl alcohol, the amount of absolute ethyl alcohol gets final product mixed-powder all can be immersed, carried out magnetic agitation 3 hours, 150～200 rev/mins of speeds of agitator, with the 100W ultrasonic wave mixed system was processed 1 hour afterwards, removed the gas of nano-powder absorption, staticly settle 24 hours, after the abundant layering of solution system, pour out the absolute ethyl alcohol on solution upper strata, again silicone glass resin is joined in the dispersion, stir, and process with ultrasonic wave, make the nano particle Uniform Dispersion, make nano-composite coating, organic siliconresin in the nano-composite coating, the mass ratio of titanium dioxide and fluorophologopite is 48%: 39%: 13%.
Existing nylon 1010 insulator is cleaned in ultrasonic wave with alcohol, deionized water respectively, remove surface blot and greasy dirt, put at last 110 ℃ of dewatered dryings of baking oven 12 hours, the nano-composite coating that has prepared is coated to the nylon insulator surface with the method for brushing.Behind 2 hours air-dry, put into vacuum drying chamber, 60 ℃, 10
-1The vacuum degree of Pa, reducing pressure heats up solidifies, and continues 12 hours, finally makes the nylon 1010 insulator with Nanosurface composite coating.
The nylon 1010 insulator that will have nano-composite coating is tested, test result as shown in Figure 4, Reference numeral 5 is for being coated with the nylon 1010 insulator of nano-composite coating, Reference numeral 4 is nylon 1010 insulator matrix.As shown in Figure 4, existing nylon insulator is in the tri compound coating of surperficial clad nano titanium dioxide-organosilicon-mica, fall is 50% approximately, and theoretical according to the field strength distribution at three binding site places, the decline of dielectric constant can significantly improve its insulation property under vacuum condition.
The vacuum flashover voltage of pure nylon 1010 insulator is 191.45kV.Vacuum insulation flashover performance table with test results is bright, and the vacuum flashover voltage of the nylon insulator behind the coated with nano composite coating is improved, and data see Table 1.
Embodiment 2:
Preparation technology such as embodiment 1, difference is, the mass percent of silicone glass resin, nano titanium oxide and fluorophologopite 68%: 24%: 8%, 200～250 rev/mins of speeds of agitator; Vacuum insulation flashover performance table with test results is bright, and the vacuum flashover voltage of the nylon insulator behind the coated with nano composite coating is improved, and data see Table 1.
Embodiment 3:
Preparation technology such as embodiment 1, difference is, the mass percent of silicone glass resin, nano titanium oxide and fluorophologopite is 53%: 35%: 12%, vacuum insulation flashover performance table with test results is bright, the vacuum flashover voltage of the nylon insulator behind the coated with nano composite coating is improved, and data see Table 1.
Embodiment 4:
Preparation technology such as embodiment 1, difference is that the mass percent of silicone glass resin, nano titanium oxide and fluorophologopite is 62%: 28.5%: 9.5%, 200～250 rev/mins of speeds of agitator; Vacuum insulation flashover performance table with test results is bright, and the vacuum flashover voltage of the nylon insulator behind the coated with nano composite coating is improved, and data see Table 1.
Table 1
Claims (5)
1. vacuum composite insulating material, comprise nylon 1010 insulator basis material and nano-composite coating, described nano-composite coating comprises organic siliconresin, nano titanium oxide and fluorophologopite, the content of described organic siliconresin is 40 ~ 75wt%, the content of nano titanium oxide is 20 ~ 40wt%, and the content of fluorophologopite is 5 ~ 20wt%.
2. vacuum composite insulating material according to claim 1 is characterized in that, the content of described organic siliconresin is 50 ~ 70wt%, and the content of nano titanium oxide is 25 ~ 40wt%, and the content of fluorophologopite is 8 ~ 13wt%.
3. vacuum composite insulating material according to claim 1 and 2 is characterized in that, described organic siliconresin is silicone glass resin.
One kind prepare according to claim 1 ~ 3 in the technique of the described vacuum composite insulating material of any one, comprising:
A) utilize solvent-ultrasonic wave dispersion method to prepare nano-composite coating: first nano titanium oxide and fluorophologopite dried bean noodles is dry, mixing, in anhydrous solvent, stir, carry out ultrasonic wave and process; And then the adding organic siliconresin, stir and carry out ultrasonic wave and process;
B) nano-composite coating of above-mentioned preparation is coated in the surface of nylon 1010 insulator basis material, and solidifies.
5. technique according to claim 4 is characterized in that, described solvent is ethanol, and the temperature of described curing is 60 ~ 90 ℃.
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| CN105331046B (en) * | 2015-11-16 | 2018-07-17 | 国家纳米科学中心 | A kind of direct-current ultra high voltage insulator, preparation method and its usage |
| CN106057381B (en) * | 2016-05-19 | 2017-10-03 | 国网河南省电力公司南阳供电公司 | A kind of multifunctional colour porcelain insulator |
| CN110189874A (en) * | 2019-05-28 | 2019-08-30 | 华中科技大学 | A kind of preparation method of the insulator based on 3D printing technique |
| CN113053594B (en) * | 2021-03-16 | 2022-10-28 | 江西省萍乡市南溪电瓷电器制造有限公司 | Antifouling type clavate suspension type porcelain insulator and preparation method thereof |
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| CN101709163A (en) * | 2009-10-28 | 2010-05-19 | 北京航空航天大学 | Organic/inorganic silicon hybridization water-based anti-corrosion paint applicable to magnesium alloy surface and preparation method thereof |
| CN101800099A (en) * | 2009-02-06 | 2010-08-11 | 上海均达科技发展有限公司 | Mica insulator |
| CN101967335A (en) * | 2010-10-09 | 2011-02-09 | 青岛爱尔家佳新材料有限公司 | Breakdown-resistant insulating paint |
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Patent Citations (5)
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| CN1877751A (en) * | 2006-07-03 | 2006-12-13 | 上海电气集团股份有限公司 | Pollution flashover preventing insulator |
| CN101800099A (en) * | 2009-02-06 | 2010-08-11 | 上海均达科技发展有限公司 | Mica insulator |
| CN201425867Y (en) * | 2009-05-18 | 2010-03-17 | 沪东中华造船(集团)有限公司 | Insulating porcelain bottle for high-hanging slide line |
| CN101709163A (en) * | 2009-10-28 | 2010-05-19 | 北京航空航天大学 | Organic/inorganic silicon hybridization water-based anti-corrosion paint applicable to magnesium alloy surface and preparation method thereof |
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