CN103121847B - A kind of preparation method of SiBON electromagnetic wave transparent materials - Google Patents
A kind of preparation method of SiBON electromagnetic wave transparent materials Download PDFInfo
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- CN103121847B CN103121847B CN201310026180.6A CN201310026180A CN103121847B CN 103121847 B CN103121847 B CN 103121847B CN 201310026180 A CN201310026180 A CN 201310026180A CN 103121847 B CN103121847 B CN 103121847B
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Abstract
The present invention relates to a kind of preparation method of SiBON electromagnetic wave transparent materials, belong to aeronautical material technical field.It is characterized in that using tetraethyl orthosilicate, boric acid, metallic silicon power as raw material, SiBON powder body materials are prepared using metallic silicon power reduction, obtained powder is recycled to prepare SiBON ceramic materials, realize that dielectric properties are excellent, stable mechanical property electromagnetic wave transparent material, for the update of radome material, provide and provide powerful support for for the development of space flight and aviation cause.There is reference to the performance for studying SiBON materials from now on.
Description
Technical field
The present invention relates to a kind of preparation method of SiBON electromagnetic wave transparent materials, belong to aeronautical material technical field.
Background technology
In recent years, as the serial airship in Divine Land constantly goes up to the air, China's space flight and aviation cause is flourished, and all kinds of aviations are navigated
The demand of its material is increasing.Wherein, electromagnetic wave transparent material is the key factor for restricting aeronautical and space technology development.Electromagnetic wave transparent material is
The material of wavelength electromagnetic wave within 1-1000mm scopes can be passed through by referring to, and transmitance requirement reaches 70%.To ensure internal device
Part can normal work, electromagnetic wave transparent material requirement have preferable dielectric properties, intensity, fracture toughness, thermal shock resistance and resistance to punching
Lose polishing machine.
At present, electromagnetic wave transparent material mainly has following several：Polymer matrix composites, alumina ceramic material, devitrified glass material
Material, silicon dioxide body based material, phosphate material, nitride ceramics etc..The temperature in use scope of polymer matrix composites
Generally 100 DEG C -400 DEG C, but high temperature strength is relatively low, it is impossible to applied on the aircraft of high-speed flight；With silica
There is good thermal shock resistance for the electromagnetic wave transparent material of matrix, dielectric constant is also relatively low, be conducive to the reception of the signal of inside antenna, but
It is that its room temperature strength is not high；There is higher heat endurance using nitride as the electromagnetic wave transparent material of matrix, bending strength can also reach
To between 100MPa-200MPa, dielectric constant is 7-9, and the signal for being unfavorable for inside antenna is received.Although the species of electromagnetic wave transparent material
It is various, but it is also fewer suitable for the electromagnetic wave transparent material of hypersonic vehicle at present.
Boron nitride ceramics electromagnetic wave transparent material has the advantages that intensity, toughness are higher and dielectric constant is relatively low, but in height
Wave transmission rate under temperature is substantially reduced, it is impossible to meet the condition used under high temperature；Quartz-ceramics electromagnetic wave transparent material properties all compare
Equilibrium, but erosive resistance is poor, constrains its application.Therefore, Si-B-O-N materials are used as a kind of Novel wave material
The study hotspot of material, not only maintains SiO2With the advantage of BN superior dielectric performances, and make its mechanical property in different temperatures
It is lower to keep stable.The development of Si-B-O-N materials is divided into two steps：More ripe SiO2With BN composites and big
The SiBON materials of power research.
Therefore, the present invention is on the basis of SiBON investigations of materials, it is proposed that a kind of novel processing step of SiBON materials.
After the gel drying of tetraethyl orthosilicate and acid reaction, using metallic silicon power high temperature reduction in a nitrogen atmosphere, SiBON is prepared
Powder, powder is sintered in protective atmosphere preparation SiBON ceramic materials.This method is for preparing high-performance SiBON wave transparent materials
Material has important Research Significance.
The content of the invention
The present invention is on the basis of for SiBON investigations of materials, it is proposed that a kind of novel processing step of SiBON materials.
By controlling the temperature and soaking time of the consumption of tetraethyl orthosilicate and boric acid, the addition of metallic silicon power and pressureless sintering to control
Course of reaction processed, obtains SiBON powder body materials, then obtains SiBON base substrates using dry pressing, and enter in a nitrogen atmosphere
Row high-temperature calcination, prepares SiBON electromagnetic wave transparent materials.The present invention is with product purity is high, dielectric properties are excellent, mechanical property is steady
The advantages of determining, is widely used in Aero-Space cause in the electromagnetic wave transparent material such as antenna house.
A kind of novel processing step of SiBON materials proposed by the present invention.It is characterized in that：With tetraethyl orthosilicate, boric acid,
Metallic silicon power is raw material, and tetraethyl orthosilicate is slowly added dropwise into boric acid solution, water-bath magnetic agitation, is settled into after being added dropwise to complete
Gel.Dried in 120 DEG C of thermostatic drying chambers, xerogel and metallic silicon power are carried out into dispensing, ball milling, dry pressuring forming process prepares
Base substrate, in N2Under atmosphere, 2h-6h is incubated at a temperature of 1100 DEG C -1500 DEG C, it is taking-up grinding and mistake after room temperature to be cooled to
200 mesh sieves, obtain SiBON powders.Powder is dry-pressing formed, and briquetting pressure is 5MPa-30MPa, and isostatic cool pressing pressure is
150MPa-200MPa, the dwell time is 10s-90s.By base substrate be put into nitrogen protection atmosphere furnace in, programming rate be 5 DEG C/
Min, after insulation 1h-10h at a temperature of 1400 DEG C -1700 DEG C, SiBON materials can be obtained by naturally cooling to after room temperature.
The method that a kind of high temperature solid-state method proposed by the present invention prepares SiBON materials, described technological process is specially：
1) tetraethyl orthosilicate is slowly added dropwise into 1%-4.5% boric acid solution, done using sodium dodecylbenzenesulfonate
Surfactant, is stirred under 80 DEG C of water baths, stands plastic.Gel is placed in 120 DEG C of thermostatic drying chambers and dried,
It is stand-by that xerogel is levigate.
2) planetary ball is loaded in chemical equation ratio dispensing using 10 μm~45 μm metallic silicon powers and above-mentioned xerogel
Dry grinded in grinding machine, particle diameter 1h-24h is uniform to stock dispersion.
3) raw material is dry-pressing formed, in the atmosphere furnace that base substrate is put into nitrogen protection, programming rate is 1~10 DEG C/min,
It is incubated to naturally cool to after 2h-6h at 1100 DEG C~1500 DEG C and is taken out after room temperature, grinds and cross 200 mesh sieves.
4) obtained powder is dry-pressing formed, pressure is 5MPa-30MPa, and the dwell time is 60s.Sample is carried out again cold
Isostatic pressed, pressure is 150MPa-200MPa, and the dwell time is 60s.
5) base substrate is put into the atmosphere furnace of nitrogen protection, programming rate is 5 DEG C/min, in 1400 DEG C of -1700 DEG C of temperature
Lower sintering, and 1h-10h is incubated, SiBON materials can be obtained by naturally cooling to after room temperature.
The present invention proposes a kind of method that pressureless sintering prepares SiBON materials.By controlling tetraethyl orthosilicate and boric acid
Consumption, the addition of metallic silicon power and the temperature of pressureless sintering and soaking time control course of reaction, purity can be obtained
High, dielectric properties are excellent, stable mechanical property SiBON materials, can apply in the electromagnetic wave transparent materials such as antenna house, promote boat
The development of empty aerospace industry.
Embodiment
Embodiment 1：
The material composition and granularity requirements that high temperature prepares SiBON electromagnetic wave transparent materials be：Tetraethyl orthosilicate, the quality of silica
Fraction is 48.0%-50.0%；Boric acid, is analyzed pure；Deionized water；Metallic silicon power, 45 μ n；High pure nitrogen.
According to Si-B than calculating tetraethyl orthosilicate addition, tetraethyl orthosilicate is slowly added dropwise into 3% boric acid solution,
Surfactant is made using sodium dodecylbenzenesulfonate, in 80 DEG C of water-bath magnetic agitations, plastic is stood after being added dropwise to complete.By gel
It is placed in 120 DEG C of dryings in thermostatic drying chamber.Load planetary by both certainty ratio dispensings with 45 μm of metallic silicon powers after xerogel is levigate
The 12h that dry grinded in ball mill is uniform to stock dispersion.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection
In, programming rate is 5 DEG C/min, is incubated at 1100 DEG C after 6h and naturally cools to room temperature, grinds and crosses 200 mesh sieves, obtains
SiBON powder body materials.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carries out isostatic cool pressing, and pressure is 200MPa,
Dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, programming rate is insulation at 5 DEG C/min, 1500 DEG C
Taken out after 6h, natural cooling and obtain SiBON materials.
The SiBON materials prepared by above-described embodiment 1, its strength at normal temperature value is 180MPa, and dielectric constant is
3.2。
Embodiment 2：
The material composition and granularity requirements that high temperature prepares SiBON electromagnetic wave transparent materials be：Tetraethyl orthosilicate, the quality of silica
Fraction is 48.0%-50.0%；Boric acid, is analyzed pure；Deionized water；Metallic silicon power, 45 μm；High pure nitrogen.
According to Si-B than calculating tetraethyl orthosilicate addition, tetraethyl orthosilicate is slowly added dropwise into 3% boric acid solution,
Surfactant is made using sodium dodecylbenzenesulfonate, in 80 DEG C of water-bath magnetic agitations, plastic is stood after being added dropwise to complete.By gel
It is placed in 120 DEG C of dryings in thermostatic drying chamber.Load planetary by both certainty ratio dispensings with 45 μm of metallic silicon powers after xerogel is levigate
The 12h that dry grinded in ball mill is uniform to stock dispersion.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection
In, programming rate is 5 DEG C/min, is incubated at 1200 DEG C after 6h and naturally cools to room temperature, grinds and crosses 200 mesh sieves, obtains
SiBON powder body materials.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carries out isostatic cool pressing, and pressure is 200MPa,
Dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, programming rate is insulation at 5 DEG C/min, 1500 DEG C
Taken out after 6h, natural cooling and obtain SiBON materials.
The SiBON materials prepared by above-described embodiment 2, its strength at normal temperature value is 187MPa, and dielectric constant is
3.3。
Embodiment 3：
The material composition and granularity requirements that high temperature prepares SiBON electromagnetic wave transparent materials be：Tetraethyl orthosilicate, the quality of silica
Fraction is 48.0%-50.0%；Boric acid, is analyzed pure；Deionized water；Metallic silicon power, 45 μm；High pure nitrogen.
According to Si-B than calculating tetraethyl orthosilicate addition, tetraethyl orthosilicate is slowly added dropwise into 3% boric acid solution,
Surfactant is made using sodium dodecylbenzenesulfonate, in 80 DEG C of water-bath magnetic agitations, plastic is stood after being added dropwise to complete.By gel
It is placed in 120 DEG C of dryings in thermostatic drying chamber.Load planetary by both certainty ratio dispensings with 45 μm of metallic silicon powers after xerogel is levigate
The 12h that dry grinded in ball mill is uniform to stock dispersion.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection
In, programming rate is 5 DEG C/min, is incubated at 1300 DEG C after 6h and naturally cools to room temperature, grinds and crosses 200 mesh sieves, obtains
SiBON powder body materials.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carries out isostatic cool pressing, and pressure is 200MPa,
Dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, programming rate is insulation at 5 DEG C/min, 1500 DEG C
Taken out after 6h, natural cooling and obtain SiBON materials.
The SiBON materials prepared by above-described embodiment 3, its strength at normal temperature value is 197MPa, and dielectric constant is
3.1。
Embodiment 4：
The material composition and granularity requirements that high temperature prepares SiBON electromagnetic wave transparent materials be：Tetraethyl orthosilicate, the quality of silica
Fraction is 48.0%-50.0%；Boric acid, is analyzed pure；Deionized water；Metallic silicon power, 45 μm；High pure nitrogen.
According to Si-B than calculating tetraethyl orthosilicate addition, tetraethyl orthosilicate is slowly added dropwise into 3% boric acid solution,
Surfactant is made using sodium dodecylbenzenesulfonate, in 80 DEG C of water-bath magnetic agitations, plastic is stood after being added dropwise to complete.By gel
It is placed in 120 DEG C of dryings in thermostatic drying chamber.Load planetary by both certainty ratio dispensings with 45 μm of metallic silicon powers after xerogel is levigate
The 12h that dry grinded in ball mill is uniform to stock dispersion.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection
In, programming rate is 5 DEG C/min, is incubated at 1400 DEG C after 6h and naturally cools to room temperature, grinds and crosses 200 mesh sieves, obtains
SiBON powder body materials.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carries out isostatic cool pressing, and pressure is 200MPa,
Dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, programming rate is insulation at 5 DEG C/min, 1500 DEG C
Taken out after 6h, natural cooling and obtain SiBON materials.
The SiBON materials prepared by above-described embodiment 4, its strength at normal temperature value is 192MPa, and dielectric constant is
3.1。
Embodiment 5：
The material composition and granularity requirements that high temperature prepares SiBON electromagnetic wave transparent materials be：Tetraethyl orthosilicate, the quality of silica
Fraction is 48.0%-50.0%；Boric acid, is analyzed pure；Deionized water；Metallic silicon power, 45 μm；High pure nitrogen.
According to Si-B than calculating tetraethyl orthosilicate addition, tetraethyl orthosilicate is slowly added dropwise into 3% boric acid solution,
Surfactant is made using sodium dodecylbenzenesulfonate, in 80 DEG C of water-bath magnetic agitations, plastic is stood after being added dropwise to complete.By gel
It is placed in 120 DEG C of dryings in thermostatic drying chamber.Load planetary by both certainty ratio dispensings with 45 μm of metallic silicon powers after xerogel is levigate
The 12h that dry grinded in ball mill is uniform to stock dispersion.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection
In, programming rate is 5 DEG C/min, is incubated at 1500 DEG C after 6h and naturally cools to room temperature, grinds and crosses 200 mesh sieves, obtains
SiBON powder body materials.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carries out isostatic cool pressing, and pressure is 200MPa,
Dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, programming rate is insulation at 5 DEG C/min, 1500 DEG C
Taken out after 6h, natural cooling and obtain SiBON materials.
The SiBON materials prepared by above-described embodiment 5, its strength at normal temperature value is 198MPa, and dielectric constant is
2.9。
Claims (1)
1. a kind of preparation method of SiBON materials, it is characterised in that comprise the following steps：
Step 1) using tetraethyl orthosilicate, boric acid, metallic silicon power as raw material, boric acid is dissolved in deionized water and forms boric acid solution,
Tetraethyl orthosilicate is slowly added dropwise into boric acid solution, done using sodium dodecylbenzenesulfonate under surfactant, water bath
It is stirred, stands plastic；
Step 2) gel is placed in 120 DEG C of thermostatic drying chambers and dried, xerogel is levigate, and rear and metallic silicon power carries out dispensing, ball
Mill, dry pressuring forming process prepare base substrate, in N2Lower 1100 DEG C of -1500 DEG C of calcinings of atmosphere, are incubated after 2h -6h, natural cooling and take out,
Grind and cross 200 mesh sieves and obtain SiBON powder body materials；
Step 3) powder is dry-pressing formed, obtained base substrate is put into N2In the atmosphere furnace of atmosphere protection, programming rate is 5 DEG C/min,
SiBON materials can be obtained by naturally cooling to room temperature after insulation 1h-10h at 1400 DEG C -1700 DEG C.
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