CN105859270A - Preparation method of high-temperature-resistant compound wave-transmitting material - Google Patents
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- CN105859270A CN105859270A CN201610208978.6A CN201610208978A CN105859270A CN 105859270 A CN105859270 A CN 105859270A CN 201610208978 A CN201610208978 A CN 201610208978A CN 105859270 A CN105859270 A CN 105859270A
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Abstract
The invention relates to a preparation method of a high-temperature-resistant compound wave-transmitting material and belongs to the technical field of preparation of wave-transmitting materials. The invention aims at solving the problems that an existing prepared wave-transmitting material is mainly a silicon dioxide composite wave-transmitting material, crystallization is caused at high temperature and strength is reduced; and the method provided by the invention comprises the following steps of: compounding tetraethyl orthosilicate with ethanol to prepare ageing solution, then compounding the ageing solution with magnesium oxide talcum powder and ammonium hydrogen carbonate to prepare gel, calcining and milling to prepare cordierite ceramic powder, preparing a wave-transmitting material from the cordierite ceramic powder instead of silicon dioxide, effectively improving heat resistance of the wave-transmitting material, then compounding the wave-transmitting material with silicon nitride and boron silicon to prepare a wave-transmitting material. The prepared high-temperature-resistant wave-transmitting material is obviously improved in high temperature resistance, bending strength at the temperature of 1000 DEG C can reach 180MPa, coefficient of thermal expansion is 2.0*10<-6>/DEG C<-1>, and a preparation process is simple and green and pollution-free to the environment.
Description
Technical field
The present invention relates to the preparation method of a kind of high temperature resistant compound electromagnetic wave transparent material, belong to wave transparent preparing technical field.
Background technology
Electromagnetic wave transparent material refers to wavelength one; frequency is in a range and the transmitance of electromagnetic wave is more than; can be used in protecting aerospace craft communication in the presence of a harsh environment, remote measurement, guide, a kind of Multifunctional nursing material that the system such as ignition can normally work, in the fields such as carrier rocket, airship, guided missile and retrievable satellite, be widely applied one.Different working environments residing for aircraft are different, and the radio of use is the most different, thus the requirement to electromagnetic wave transparent material is widely different.Space flight electromagnetic wave transparent material is broadly divided into antenna windows and the big class of antenna house two by the form of its structural member; wherein antenna windows is normally at the side of aircraft; usually flat board or the tabular of band cambered surface; mainly for the protection of the radio after antenna windows; make it normally can be positioned at the head of aircraft by working day irdome in the presence of a harsh environment, mostly be taper, the most also have hemispherical; having the several functions such as water conservancy diversion, solar heat protection, wave transparent, carrying, its performance requirement is higher than the former.
But existing electromagnetic wave transparent material is due to more and more higher to the requirement of temperature, the temperature that existing electromagnetic wave transparent material can bear is relatively low, its demand to product cannot be met, this is mainly due to the electromagnetic wave transparent material of preparation, mainly silicon dioxide is combined electromagnetic wave transparent material, quartz fibre is when more than 800 DEG C, make intensity decline rapidly because of crystallize, when temperature is more than 1200 C, grow up due to crystal grain and cause loss of strength totally, it is less to the ability to bear of its temperature, it is impossible to meet the demand of current material, so it is necessary to need to prepare a kind of resistant to elevated temperatures electromagnetic wave transparent material.
Summary of the invention
The technical problem to be solved: for the electromagnetic wave transparent material of preparation at present, mainly silicon dioxide is combined electromagnetic wave transparent material, at high temperature, cause its crystallize the problem making its intensity decline, provide a kind of by by compound to tetraethyl orthosilicate and ethanol preparation ageing liquid, gel is prepared again by compound with magnesium oxide Pulvis Talci and ammonium hydrogen carbonate for ageing liquid, milled by calcining and prepare cordierite ceramic powder, silicon dioxide is replaced to be prepared electromagnetic wave transparent material by standby cordierite ceramic powder, it is effectively improved electromagnetic wave transparent material heat resistanceheat resistant performance, pass through it again and silicon nitride is combined with boron nitride and prepares electromagnetic wave transparent material, its high-temperature capability and thermal shock resistance significantly improve.
Solving above-mentioned technical problem, the present invention uses the technical scheme as described below to be:
(1) count by weight, weigh 35～50 parts of tetraethyl orthosilicates, 15～20 parts of dehydrated alcohol and 35～45 parts of distilled water respectively in there-necked flask, stirring mixing also regulates pH to 2.5 with mass concentration 15% salpeter solution, continue thereafter with stirring mixing 25～30min, at 25～35 DEG C, it is aged 24h, is prepared into ageing liquid；
(2) count the most by weight, the ethanol solution choosing the ageing liquid of 25～45 parts of above-mentioned preparations, 15～20 parts of ammonium hydrogen carbonate, 10～15 parts of magnesium oxide and 10～15 parts of Pulvis Talci and 20～25 parts of mass concentrations 45% respectively is placed in there-necked flask, water-bath preheating 25～30min at 65～70 DEG C, after preheating completes, then it is placed on heating in water bath 45～60min at 85～100 DEG C；
(3) after heating in water bath completes, stop heating and it is filtered, collect upper strata filtrate rotary evaporated to dryness, it is subsequently placed in Muffle furnace, it is warming up to 450～500 DEG C by the rate program of 8 DEG C/min, heat preservation sintering 1～2h, stops heating subsequently and standing is cooled to 20～30 DEG C, and milling it is prepared into cordierite ceramic powder；
(4) count by weight, choose the cordierite ceramic powder of 25～45 parts of above-mentioned preparations, 25～30 parts of silicon nitrides, 10～15 parts of Cs2Os and 20～30 parts of boron nitride particles respectively to be placed in cylinder of steel, with dehydrated alcohol as dispersant, zirconium oxide is ball milling pearl, it is carried out ball milling, controlling ball milling speed is 200～250r/min so that it is ball milling 6～8h；
(5) after ball milling completes, 1:5 in mass ratio, gamma-aminopropyl-triethoxy-silane is added in the powder that extremely above-mentioned ball milling completes, it is again placed in ball grinder, ball milling 3～5h is continued by above-mentioned steps, it is subsequently placed at 65～80 DEG C and is dried 6～8h and it is sieved, be prepared into 60～80 mesh modified powders；
(6) 1:3 in mass ratio, cordierite powder modified powder and the step (3) of above-mentioned preparation prepared stirring mixes, and is again placed in ball grinder, and control polyvinyl alcohol is dispersant, to its ball milling and mill, is prepared into mixed-powder；
(7) mixed-powder of above-mentioned preparation is placed in graphite jig, compacting is placed in vacuum hotpressing stove, its logical nitrogen is got rid of air, the most in a nitrogen atmosphere, being heated to 1600 DEG C by 10 DEG C/min ramp, loading uniaxial tension is 30MPa, to its Heat preservation 1～2h, stop heating subsequently and standing is cooled to 20～30 DEG C, a kind of high temperature resistant compound electromagnetic wave transparent material can be prepared into.
High temperature resistant wave-permeable material density of material 2.0g/cm prepared by the present invention2, bending strength is up to 180.5MPa, and relative dielectric constant is 5.5～6.0.
The present invention is compared with additive method, and Advantageous Effects is:
(1) the high temperature resistant wave-permeable material resistance to elevated temperatures that prepared by the present invention significantly improves, and 1000 DEG C of flexural strengths are up to 180MPa, and thermal coefficient of expansion is 2.0 × 10-6/℃-1；
(2) preparation process of the present invention is simple, environmental protection, environmentally safe.
Detailed description of the invention
Count the most by weight, weigh 35～50 parts of tetraethyl orthosilicates, 15～20 parts of dehydrated alcohol and 35～45 parts of distilled water respectively in there-necked flask, stirring mixing also regulates pH to 2.5 with mass concentration 15% salpeter solution, continue thereafter with stirring mixing 25～30min, at 25～35 DEG C, it is aged 24h, is prepared into ageing liquid；Count the most by weight, the ethanol solution choosing the ageing liquid of 25～45 parts of above-mentioned preparations, 15～20 parts of ammonium hydrogen carbonate, 10～15 parts of magnesium oxide and 10～15 parts of Pulvis Talci and 20～25 parts of mass concentrations 45% respectively is placed in there-necked flask, water-bath preheating 25～30min at 65～70 DEG C, after preheating completes, then it is placed on heating in water bath 45～60min at 85～100 DEG C；After heating in water bath completes, stop heating and it is filtered, collect upper strata filtrate rotary evaporated to dryness, it is subsequently placed in Muffle furnace, it is warming up to 450～500 DEG C by the rate program of 8 DEG C/min, heat preservation sintering 1～2h, stops heating subsequently and standing is cooled to 20～30 DEG C, and milling it is prepared into cordierite ceramic powder；Count by weight, choose the cordierite ceramic powder of 25～45 parts of above-mentioned preparations, 25～30 parts of silicon nitrides, 10～15 parts of Cs2Os and 20～30 parts of boron nitride particles respectively to be placed in cylinder of steel, with dehydrated alcohol as dispersant, zirconium oxide is ball milling pearl, it is carried out ball milling, controlling ball milling speed is 200～250r/min so that it is ball milling 6～8h；After ball milling completes, 1:5 in mass ratio, gamma-aminopropyl-triethoxy-silane is added in the powder that extremely above-mentioned ball milling completes, it is again placed in ball grinder, ball milling 3～5h is continued by above-mentioned steps, it is subsequently placed at 65～80 DEG C and is dried 6～8h and it is sieved, be prepared into 60～80 mesh modified powders；1:3 in mass ratio, mixes the stirring of the modified powder of above-mentioned preparation and cordierite powder, and is again placed in ball grinder, and control polyvinyl alcohol is dispersant, to its ball milling and mill, is prepared into mixed-powder；The mixed-powder of above-mentioned preparation is placed in graphite jig, compacting is placed in vacuum hotpressing stove, its logical nitrogen is got rid of air, the most in a nitrogen atmosphere, being heated to 1600 DEG C by 10 DEG C/min ramp, loading uniaxial tension is 30MPa, to its Heat preservation 1～2h, stop heating subsequently and standing is cooled to 20～30 DEG C, a kind of high temperature resistant compound electromagnetic wave transparent material can be prepared into.
Example 1
Count the most by weight, 35 parts of tetraethyl orthosilicates of weighing, 20 parts of dehydrated alcohol and 45 parts of distilled water are in there-necked flask respectively, and stirring mixing also regulates pH to 2.5 with mass concentration 15% salpeter solution, continue thereafter with stirring and mix 25min, at 25 DEG C, it is aged 24h, is prepared into ageing liquid；Count the most by weight, the ethanol solution choosing the ageing liquid of 25 parts of above-mentioned preparations, 20 parts of ammonium hydrogen carbonate, 15 parts of magnesium oxide and 15 parts of Pulvis Talci and 25 parts of mass concentrations 45% respectively is placed in there-necked flask, water-bath preheating 25min at 65 DEG C, after preheating completes, then it is placed on heating in water bath 45min at 850 DEG C；After heating in water bath completes, stop heating and it is filtered, collect upper strata filtrate rotary evaporated to dryness, it is subsequently placed in Muffle furnace, it is warming up to 450 DEG C by the rate program of 8 DEG C/min, heat preservation sintering 1h, stops heating subsequently and standing is cooled to 20 DEG C, and milling it is prepared into cordierite ceramic powder；Count by weight, choose the cordierite ceramic powder of 30 parts of above-mentioned preparations, 30 parts of silicon nitrides, 10 parts of Cs2Os and 30 parts of boron nitride particles respectively to be placed in cylinder of steel, with dehydrated alcohol as dispersant, zirconium oxide is ball milling pearl, it is carried out ball milling, controlling ball milling speed is 225r/min so that it is ball milling 7h；After ball milling completes, 1:5 in mass ratio, adds in the powder that extremely above-mentioned ball milling completes by gamma-aminopropyl-triethoxy-silane, it is again placed in ball grinder, continue ball milling 4h by above-mentioned steps, be subsequently placed at 70 DEG C and be dried 7h and it is sieved, be prepared into 70 mesh modified powders；1:3 in mass ratio, mixes the stirring of the modified powder of above-mentioned preparation and cordierite powder, and is again placed in ball grinder, and control polyvinyl alcohol is dispersant, to its ball milling and mill, is prepared into mixed-powder；The mixed-powder of above-mentioned preparation is placed in graphite jig, compacting is placed in vacuum hotpressing stove, its logical nitrogen is got rid of air, the most in a nitrogen atmosphere, being heated to 1600 DEG C by 10 DEG C/min ramp, loading uniaxial tension is 30MPa, to its Heat preservation 2h, stop heating subsequently and standing is cooled to 25 DEG C, a kind of high temperature resistant compound electromagnetic wave transparent material can be prepared into.
High temperature resistant wave-permeable material density of material 2.0g/cm prepared by the present invention2, bending strength is up to 180.5MPa, and relative dielectric constant is 5.5.
Example 2
Count the most by weight, 40 parts of tetraethyl orthosilicates of weighing, 20 parts of dehydrated alcohol and 40 parts of distilled water are in there-necked flask respectively, and stirring mixing also regulates pH to 2.5 with mass concentration 15% salpeter solution, continue thereafter with stirring and mix 27min, at 27 DEG C, it is aged 24h, is prepared into ageing liquid；Count the most by weight, the ethanol solution choosing the ageing liquid of 30 parts of above-mentioned preparations, 17 parts of ammonium hydrogen carbonate, 12 parts of magnesium oxide and 12 parts of Pulvis Talci and 22 parts of mass concentrations 45% respectively is placed in there-necked flask, water-bath preheating 27min at 67 DEG C, after preheating completes, then it is placed on heating in water bath 50min at 90 DEG C；After heating in water bath completes, stop heating and it is filtered, collect upper strata filtrate rotary evaporated to dryness, it is subsequently placed in Muffle furnace, it is warming up to 470 DEG C by the rate program of 8 DEG C/min, heat preservation sintering 1h, stops heating subsequently and standing is cooled to 25 DEG C, and milling it is prepared into cordierite ceramic powder；Count by weight, choose the cordierite ceramic powder of 30 parts of above-mentioned preparations, 30 parts of silicon nitrides, 10 parts of Cs2Os and 30 parts of boron nitride particles respectively to be placed in cylinder of steel, with dehydrated alcohol as dispersant, zirconium oxide is ball milling pearl, it is carried out ball milling, controlling ball milling speed is 200r/min so that it is ball milling 7h；After ball milling completes, 1:5 in mass ratio, adds in the powder that extremely above-mentioned ball milling completes by gamma-aminopropyl-triethoxy-silane, it is again placed in ball grinder, continue ball milling 4h by above-mentioned steps, be subsequently placed at 70 DEG C and be dried 6h and it is sieved, be prepared into 60 mesh modified powders；1:3 in mass ratio, mixes the stirring of the modified powder of above-mentioned preparation and cordierite powder, and is again placed in ball grinder, and control polyvinyl alcohol is dispersant, to its ball milling and mill, is prepared into mixed-powder；The mixed-powder of above-mentioned preparation is placed in graphite jig, compacting is placed in vacuum hotpressing stove, its logical nitrogen is got rid of air, the most in a nitrogen atmosphere, being heated to 1600 DEG C by 10 DEG C/min ramp, loading uniaxial tension is 30MPa, to its Heat preservation 1h, stop heating subsequently and standing is cooled to 20 DEG C, a kind of high temperature resistant compound electromagnetic wave transparent material can be prepared into.
High temperature resistant wave-permeable material density of material 2.0g/cm prepared by the present invention2, bending strength is up to 180.5MPa, and relative dielectric constant is 5.7.
Example 3
Count the most by weight, 50 parts of tetraethyl orthosilicates of weighing, 15 parts of dehydrated alcohol and 35 parts of distilled water are in there-necked flask respectively, and stirring mixing also regulates pH to 2.5 with mass concentration 15% salpeter solution, continue thereafter with stirring and mix 30min, at 35 DEG C, it is aged 24h, is prepared into ageing liquid；Count the most by weight, the ethanol solution choosing the ageing liquid of 45 parts of above-mentioned preparations, 15 parts of ammonium hydrogen carbonate, 10 parts of magnesium oxide and 10 parts of Pulvis Talci and 20 parts of mass concentrations 45% respectively is placed in there-necked flask, water-bath preheating 30min at 70 DEG C, after preheating completes, then it is placed on heating in water bath 60min at 100 DEG C；After heating in water bath completes, stop heating and it is filtered, collect upper strata filtrate rotary evaporated to dryness, it is subsequently placed in Muffle furnace, it is warming up to 500 DEG C by the rate program of 8 DEG C/min, heat preservation sintering 2h, stops heating subsequently and standing is cooled to 30 DEG C, and milling it is prepared into cordierite ceramic powder；Count by weight, choose the cordierite ceramic powder of 45 parts of above-mentioned preparations, 25 parts of silicon nitrides, 10 parts of Cs2Os and 20 parts of boron nitride particles respectively to be placed in cylinder of steel, with dehydrated alcohol as dispersant, zirconium oxide is ball milling pearl, it is carried out ball milling, controlling ball milling speed is 250r/min so that it is ball milling 8h；After ball milling completes, 1:5 in mass ratio, adds in the powder that extremely above-mentioned ball milling completes by gamma-aminopropyl-triethoxy-silane, it is again placed in ball grinder, continue ball milling 5h by above-mentioned steps, be subsequently placed at 80 DEG C and be dried 8h and it is sieved, be prepared into 80 mesh modified powders；1:3 in mass ratio, mixes the stirring of the modified powder of above-mentioned preparation and cordierite powder, and is again placed in ball grinder, and control polyvinyl alcohol is dispersant, to its ball milling and mill, is prepared into mixed-powder；The mixed-powder of above-mentioned preparation is placed in graphite jig, compacting is placed in vacuum hotpressing stove, its logical nitrogen is got rid of air, the most in a nitrogen atmosphere, being heated to 1600 DEG C by 10 DEG C/min ramp, loading uniaxial tension is 30MPa, to its Heat preservation 2h, stop heating subsequently and standing is cooled to 30 DEG C, a kind of high temperature resistant compound electromagnetic wave transparent material can be prepared into.
High temperature resistant wave-permeable material density of material 2.0g/cm prepared by the present invention2, bending strength is up to 180.5MPa, and relative dielectric constant is 6.0.
Claims (1)
1. the preparation method of a high temperature resistant compound electromagnetic wave transparent material, it is characterised in that concrete preparation process is:
(1) count by weight, weigh 35～50 parts of tetraethyl orthosilicates, 15～20 parts of dehydrated alcohol and 35～45 parts of distilled water respectively in there-necked flask, stirring mixing also regulates pH to 2.5 with mass concentration 15% salpeter solution, continue thereafter with stirring mixing 25～30min, at 25～35 DEG C, it is aged 24h, is prepared into ageing liquid；
(2) count the most by weight, the ethanol solution choosing the ageing liquid of 25～45 parts of above-mentioned preparations, 15～20 parts of ammonium hydrogen carbonate, 10～15 parts of magnesium oxide and 10～15 parts of Pulvis Talci and 20～25 parts of mass concentrations 45% respectively is placed in there-necked flask, water-bath preheating 25～30min at 65～70 DEG C, after preheating completes, then it is placed on heating in water bath 45～60min at 85～100 DEG C；
(3) after heating in water bath completes, stop heating and it is filtered, collect upper strata filtrate rotary evaporated to dryness, it is subsequently placed in Muffle furnace, it is warming up to 450～500 DEG C by the rate program of 8 DEG C/min, heat preservation sintering 1～2h, stops heating subsequently and standing is cooled to 20～30 DEG C, and milling it is prepared into cordierite ceramic powder；
(4) count by weight, choose the cordierite ceramic powder of 25～45 parts of above-mentioned preparations, 25～30 parts of silicon nitrides, 10～15 parts of Cs2Os and 20～30 parts of boron nitride particles respectively to be placed in cylinder of steel, with dehydrated alcohol as dispersant, zirconium oxide is ball milling pearl, it is carried out ball milling, controlling ball milling speed is 200～250r/min so that it is ball milling 6～8h；
(5) after ball milling completes, 1:5 in mass ratio, gamma-aminopropyl-triethoxy-silane is added in the powder that extremely above-mentioned ball milling completes, it is again placed in ball grinder, ball milling 3～5h is continued by above-mentioned steps, it is subsequently placed at 65～80 DEG C and is dried 6～8h and it is sieved, be prepared into 60～80 mesh modified powders；
(6) 1:3 in mass ratio, cordierite powder modified powder and the step (3) of above-mentioned preparation prepared stirring mixes, and is again placed in ball grinder, and control polyvinyl alcohol is dispersant, to its ball milling and mill, is prepared into mixed-powder；
(7) mixed-powder of above-mentioned preparation is placed in graphite jig, compacting is placed in vacuum hotpressing stove, its logical nitrogen is got rid of air, the most in a nitrogen atmosphere, being heated to 1600 DEG C by 10 DEG C/min ramp, loading uniaxial tension is 30MPa, to its Heat preservation 1～2h, stop heating subsequently and standing is cooled to 20～30 DEG C, a kind of high temperature resistant compound electromagnetic wave transparent material can be prepared into.
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| CN201610208978.6A CN105859270A (en) | 2016-04-06 | 2016-04-06 | Preparation method of high-temperature-resistant compound wave-transmitting material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108084876A (en) * | 2017-12-12 | 2018-05-29 | 常州杰轩纺织科技有限公司 | A kind of low bulk type wave penetrating paint preparation method |
| CN108148548A (en) * | 2016-12-05 | 2018-06-12 | 航天特种材料及工艺技术研究所 | A kind of anti-weathering wave transparent antenna house of high temperature resistant and preparation method thereof |
-
2016
- 2016-04-06 CN CN201610208978.6A patent/CN105859270A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108148548A (en) * | 2016-12-05 | 2018-06-12 | 航天特种材料及工艺技术研究所 | A kind of anti-weathering wave transparent antenna house of high temperature resistant and preparation method thereof |
| CN108148548B (en) * | 2016-12-05 | 2019-11-22 | 航天特种材料及工艺技术研究所 | A kind of anti-weathering wave transparent antenna house of high temperature resistant and preparation method thereof |
| CN108084876A (en) * | 2017-12-12 | 2018-05-29 | 常州杰轩纺织科技有限公司 | A kind of low bulk type wave penetrating paint preparation method |
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Application publication date: 20160817 |