CN104058773B - A kind of synthetic method of silicic acid base electromagnetic wave transparent material - Google Patents
A kind of synthetic method of silicic acid base electromagnetic wave transparent material Download PDFInfo
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- CN104058773B CN104058773B CN201410252867.6A CN201410252867A CN104058773B CN 104058773 B CN104058773 B CN 104058773B CN 201410252867 A CN201410252867 A CN 201410252867A CN 104058773 B CN104058773 B CN 104058773B
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Abstract
The invention discloses a kind of synthetic method of silicic acid base electromagnetic wave transparent material, select quartz fiber cloth as strongthener, base-material is made with homemade inorganic sizing agent, by inorganic sizing agent and quartz fiber cloth alternately tiling, flatten, then according to certain curing process process, finally calcine, obtain silicic acid base electromagnetic wave transparent material, the silicic acid base electromagnetic wave transparent material high thermal resistance of gained of the present invention and sintering resistance can be good, and there are good mechanical property and dielectric properties, wave penetrate capability is good, can meet application needs, and preparation method is simple, synthesis condition is gentle, is convenient to implement.
Description
Technical field
The present invention relates to a kind of synthetic method of electromagnetic wave transparent material, particularly a kind of synthetic method of silicic acid base electromagnetic wave transparent material.
Background technology
High temperature wave-transparent material refers to the material being greater than 70% in 1 ~ 1000mm, frequency in the hertzian wave transmitance at sufficiently high temperature of 0.3 ~ 300GHz to wavelength.Structure electromagnetic wave transparent material system mainly contains electromagnetic wave transparent material that is high temperature resistant and normal temperature application, and the Typical Representative of this bi-material system is respectively ceramic wave-transmitting material and polymer matrix composite.Ceramic wave-transmitting material and polymer matrix composite are applied to several series products such as guided missile, aircraft radome, antenna windows and thunder radome respectively.
Due to the unstable of electromagnetic wave transparent material organic under high temperature and the characteristic of non-refractory thereof, inorganic electromagnetic wave transparent material is as the research ever more important of high temperature wave-transparent material.
Find in experiment, as inorganic electromagnetic wave transparent material-----pottery and the silicon-dioxide of electromagnetic wave transparent material, although wave penetrate capability is good, toughness is little, stress easily occurs under high temperature and breaks, with metallic seal difficulty.
Ceramic-base wave-permeation material good electric property, technique is relatively simple, and production cost is low, but material fragility is large, and damage tolerance is low, and yield rate is low.After introducing reinforced fabric, matrix material has higher damage tolerance, under exceedingly odious condition, work reliability is high, ceramic matric composite has excellent high temperature resistant electrical property, heat physical properties and mechanical behavior under high temperature, and the relatively low advanced composite material of development cost is the inexorable trend expanding electromagnetic wave transparent material Application Areas.
Summary of the invention
The invention provides a kind of synthetic method of silicic acid base electromagnetic wave transparent material, the hand that refer in organic electromagnetic wave transparent material sticks with paste technique, and obtained silicic acid base electromagnetic wave transparent material shows good wave transmission effect and resistance to elevated temperatures.
For achieving the above object, technical scheme of the present invention is as follows:
A synthetic method for silicic acid base electromagnetic wave transparent material, comprises following operation steps:
1) by a certain amount of non-hydrate sodium metasilicate and water mixing, melting under 80 ~ 100 DEG C of conditions, mix by a certain percentage with solidifying agent and additive again, stir, mix under ul-trasonic irradiation, obtained inorganic sizing agent, wherein, the weight ratio of non-hydrate sodium metasilicate, water, solidifying agent and additive is 10 ~ 15:2 ~ 3:3 ~ 5:5 ~ 10;
2) quartz fiber cloth is cut into certain shape, by above-mentioned obtained inorganic sizing agent and quartz fiber cloth alternately tiling, tiles 3 ~ 5 layers respectively, flatten, solidification treatment in the baking oven of 50 ~ 100 DEG C, leave standstill 1 ~ 5 day;
3) last, calcine in retort furnace, with the temperature rise rate of 5 ~ 10 DEG C/min, be raised to 400 ~ 800 DEG C of calcinings, insulation 2 ~ 8h.
Preferably, described solidifying agent is one or both in aluminium hydroxide, silicofluoride.
Preferably, described additive is one or more in silicon oxide, aluminum oxide, titanium dioxide, aluminum oxide, magnesium oxide or zinc oxide.
Preferably, described hyperacoustic ultrasonic frequency is 20 ~ 80KHz, and in this ultrasonic frequency range, ultrasonic effect is best.
Preferably, described solidification value is 60 ~ 80 DEG C, leaves standstill 3 ~ 4 days, and solidification value is unsuitable too high, and wants sufficiently long set time, and quartz fiber cloth and inorganic sizing agent are fully bonded together.
Preferably, during described calcining, temperature rise rate is 7 ~ 8 DEG C/min, and calcining temperature is 500 ~ 650 DEG C, and soaking time is 3 ~ 5h, strictly will control temperature rise rate during calcining, and is incubated the sufficiently long time, makes electromagnetic wave transparent material structure reach stable.
Pass through technique scheme, the synthetic method of silicic acid base electromagnetic wave transparent material provided by the invention, by resistant to elevated temperatures quartz fiber cloth as enhancing silicic acid base electromagnetic wave transparent material, with the inorganic sizing agent prepared as base-material, by inorganic sizing agent and quartz fiber cloth alternately tiling, flatten, solidify in baking oven, calcining, silicic acid base electromagnetic wave transparent material can be obtained, simple to operate, in the method, quartz fiber cloth can play the object strengthening wave penetrate capability, tiled by inorganic sizing agent and replacing of quartz fiber cloth, make structure more tight, there is higher mechanical property, the electromagnetic wave transparent material wave penetrate capability adopting the method to prepare is good, can be high temperature resistant.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below.
The SEM that Fig. 1 amplifies 10000 times for the silicic acid based composites one disclosed in the embodiment of the present invention one schemes.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below.
Embodiment one:
Quartz fiber cloth is cut into the strip of 43mm × 86mm.
Take 10g non-hydrate sodium metasilicate in beaker 1, in beaker 1, drip 2g distilled water, beaker 1 is placed in 100 DEG C of loft drier, take out after ten minutes.Take 1g Sodium Silicofluoride, 1g aluminium hydroxide and 5g silicon-dioxide, 1g pure aluminium silicate, 0.5g aluminum oxide in beaker 2, join after mixing in beaker 1 and stir 10min again, make it mix, form slurry.
Above-mentioned obtained slurry and quartz fiber cloth are alternately tiled each 3 layers, the tiling thickness of every layer of slurry is about 2mm, after 10kg pressure is flat, then one deck slurry that tiles.Be cured program: ambient temperatare puts one day, place three days under 70 DEG C of conditions, then calcine, calcination procedure is as follows: room temperature → 400 DEG C, insulation 30min → 600 DEG C, insulation 30min → 800 DEG C insulation 3h → be down to room temperature, obtained silicic acid based composites one.
Embodiment two:
Quartz fiber cloth is cut into the strip of 43mm × 86mm.
Take 15g non-hydrate sodium metasilicate in beaker 1, in beaker 1, drip 3g distilled water, beaker 1 is placed in 100 DEG C of loft drier, take out after ten minutes.Take 2g Sodium Silicofluoride, 1g aluminium hydroxide and 5g silicon-dioxide, 2g pure aluminium silicate, 3g aluminum oxide in beaker 2, join after mixing in beaker 1 and stir 10min again, make it mix, form slurry.
Above-mentioned obtained slurry and quartz fiber cloth are alternately tiled each 3 layers, the tiling thickness of every layer of slurry is about 2mm, after applying the pressing of 10kg pressure, then one deck slurry that tiles.Be cured program: ambient temperatare puts one day, place three days under 70 DEG C of conditions, then calcine, calcination procedure is as follows: room temperature → 400 DEG C, insulation 30min → 600 DEG C, insulation 30min → 800 DEG C insulation 3h → be down to room temperature, obtained silicic acid based composites two.
Embodiment three:
Quartz fiber cloth is cut into the strip of 43mm × 86mm.
Take 15g non-hydrate sodium metasilicate in beaker 1, in beaker 1, drip 3g distilled water, beaker 1 is placed in 100 DEG C of loft drier, take out after ten minutes.Take 1.5g Sodium Silicofluoride, 1.5g aluminium hydroxide and 5g silicon-dioxide, 1g pure aluminium silicate, 2g aluminum oxide in beaker 2, join after mixing in beaker 1 and stir 10min again, make it mix, form slurry.
Above-mentioned obtained slurry and quartz fiber cloth are alternately tiled each 3 layers, the tiling thickness of every layer of slurry is about 2mm, after 10kg pressure is flat, then one deck slurry that tiles.Be cured program: ambient temperatare puts one day, place three days under 70 DEG C of conditions, then calcine, calcination procedure is as follows: room temperature → 400 DEG C, insulation 30min → 600 DEG C, insulation 30min → 800 DEG C insulation 3h → be down to room temperature, obtained silicic acid based composites three.
Relative permittivity and loss tangent test:
The numerical value that employing relative permittivity tester and loss tangent tester record matrix material is as shown in table 1.
Table 1 loss tangent and relative permittivity value
| Sample name | Loss tangent | Relative permittivity |
| Silicic acid based composites one | 0.0013 | 8.1 |
| Silicic acid based composites two | 0.0015 | 8.3 |
| Silicic acid based composites three | 0.0014 | 9.0 |
| Ceramic plate | 0.0014 | 9.4 |
Data as can be seen from table 1, each material of loss tangent is all similar, but the relative permittivity of silicic acid based composites ratio pottery is less, shows that its wave penetrate capability can be better than pottery.
Electron-microscope scanning is tested:
Carry out electron-microscope scanning to the silicic acid based composites one of embodiment one gained, the SEM figure obtained is shown in Fig. 1.As can be seen from Figure 1, arrange between particle neatly compactly, be evenly distributed.
High temperature resistant test:
Sample is placed in retort furnace 1000 DEG C calcining, does not find any change.
Wave is tested:
Be positioned between magnetron and water by silicic acid based composites one, two, three and ceramic plate, open magnetron, launch light wave, the time is 1min, and the temperature rise situation of test 200g water, concrete data are in table 2.
The temperature rise situation of table 2 water
| Sample name | Water initial temperature/DEG C | Water outlet temperature/DEG C | Water temperature difference/DEG C |
| Silicic acid based composites one | 21.1 | 58.2 | 37.1 |
| Silicic acid based composites two | 20.3 | 54.8 | 34.5 |
| Silicic acid based composites three | 21.1 | 53.4 | 32.2 |
| Ceramic plate | 20.1 | 52.2 | 32.1 |
As can be seen from Table 2, light wave is after the silicic acid based composites synthesized in this programme, the temperature difference as the water of load will apparently higher than the temperature difference of water after ceramic plate, and this illustrates that the wave penetrate capability of synthetic product is better than ceramic plate, and water absorbs more ripple.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. a synthetic method for silicic acid base electromagnetic wave transparent material, is characterized in that, comprises following operation steps:
1) by a certain amount of non-hydrate sodium metasilicate and water mixing, melting under 80 ~ 100 DEG C of conditions, mix by a certain percentage with solidifying agent and additive again, stir, mix under ul-trasonic irradiation, obtained inorganic sizing agent, wherein, the weight ratio of non-hydrate sodium metasilicate, water, solidifying agent and additive is 10 ~ 15:2 ~ 3:3 ~ 5:5 ~ 10, and described solidifying agent is one or both in aluminium hydroxide, silicofluoride;
2) quartz fiber cloth is cut into certain shape, by above-mentioned obtained inorganic sizing agent and quartz fiber cloth alternately tiling, tiles 3 ~ 5 layers respectively, flatten, solidification treatment in the baking oven of 50 ~ 100 DEG C, leave standstill 1 ~ 5 day;
3) last, calcine in retort furnace, with the temperature rise rate of 5 ~ 10 DEG C/min, be raised to 400 ~ 800 DEG C of calcinings, insulation 2 ~ 8h.
2. the synthetic method of a kind of silicic acid base electromagnetic wave transparent material according to claim 1, it is characterized in that, described additive is one or more in silicon oxide, aluminum oxide, titanium dioxide, magnesium oxide or zinc oxide.
3. the synthetic method of a kind of silicic acid base electromagnetic wave transparent material according to claim 1, it is characterized in that, described hyperacoustic ultrasonic frequency is 20 ~ 80KHz.
4. the synthetic method of a kind of silicic acid base electromagnetic wave transparent material according to claim 1, it is characterized in that, described solidification value is 60 ~ 80 DEG C, leaves standstill 3 ~ 4 days.
5. the synthetic method of a kind of silicic acid base electromagnetic wave transparent material according to claim 1, is characterized in that, during described calcining, temperature rise rate is 7 ~ 8 DEG C/min, and calcining temperature is 500 ~ 650 DEG C, and soaking time is 3 ~ 5h.
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