CN103121847A - Preparation method of SiBON wave-transmitting material - Google Patents
Preparation method of SiBON wave-transmitting material Download PDFInfo
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- CN103121847A CN103121847A CN2013100261806A CN201310026180A CN103121847A CN 103121847 A CN103121847 A CN 103121847A CN 2013100261806 A CN2013100261806 A CN 2013100261806A CN 201310026180 A CN201310026180 A CN 201310026180A CN 103121847 A CN103121847 A CN 103121847A
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Abstract
The invention relates to a preparation method of a SiBON wave-transmitting material, and belongs to the technical field of an aeronautical material. The preparation method is characterized by comprising the steps of: by taking tetraethoxysilane, boric acid, and metal silicon powder as materials, reducing and preparing the SiBON powder material by using metal silicon powder; and preparing the SiBON ceramic material by using the prepared power. Thus, the wave-transmitting material with excellent dielectric property and stable mechanical property is achieved; strong support is provided for development of an aerospace career and renewal and replacement of an antenna housing material; and the preparation method has significance for research on the performance of the SiBON material in future.
Description
Technical field
The present invention relates to a kind of preparation method of SiBON electromagnetic wave transparent material, belong to the aeronautical material technical field.
Background technology
In recent years, along with Divine Land series airship constantly goes up to the air, China's space flight and aviation cause is flourish, and is increasing to the demand of all kinds of aerospace materials.Wherein, electromagnetic wave transparent material is the key factor of restriction aeronautical and space technology development.Electromagnetic wave transparent material refer to see through wavelength in the 1-1000mm scope with interior electromagnetic material, transmitance requires to reach 70%.For guaranteeing that internal components can work, electromagnetic wave transparent material requires to have dielectric properties, intensity, fracture toughness property, heat-shock resistance and erosion-wear-resisting performance preferably.
At present, electromagnetic wave transparent material mainly contains following several: polymer matrix composites, alumina ceramic material, microcrystal glass material, silicon dioxide body based material, phosphate material, nitride ceramics etc.The use temperature scope of polymer matrix composites is generally 100 ℃-400 ℃, but under high temperature, intensity is lower, can not be applied on the aircraft of high-speed flight; Electromagnetic wave transparent material take silicon-dioxide as matrix has good heat-shock resistance, and specific inductivity is also on the low side, is conducive to the reception of the signal of inside antenna, but its room temperature strength is not high; Electromagnetic wave transparent material take nitride as matrix has higher thermostability, and flexural strength also can reach between 100MPa-200MPa, and specific inductivity is 7-9, is unfavorable for that the signal of inside antenna receives.Although electromagnetic wave transparent material is of a great variety, the electromagnetic wave transparent material that is applicable at present hypersonic vehicle is also fewer.
The advantage such as the boron nitride ceramics electromagnetic wave transparent material has intensity, toughness is higher and specific inductivity is relatively low, but wave transparent rate at high temperature reduces greatly, can't satisfy the condition of using under high temperature; Quartz-ceramics electromagnetic wave transparent material properties is all more balanced, but erosive resistance is relatively poor, has restricted its application.Therefore, the Si-B-O-N material has not only kept SiO as a kind of study hotspot of Novel wave material
2With the advantage of the excellent dielectric properties of BN, and make its mechanical property keep stable under differing temps.The development of Si-B-O-N material was divided into for two steps: comparatively ripe SiO
2With the BN matrix material and energetically research the SiBON material.
Therefore, the present invention has proposed a kind of novel preparation method of SiBON material on the basis of SiBON investigation of materials.After gel drying with tetraethoxy and acid reaction, use metallic silicon power high temperature reduction under nitrogen atmosphere, preparation SiBON powder prepares the SiBON stupalith with powder sintering in protective atmosphere.The method has important Research Significance for preparation high-performance SiBON electromagnetic wave transparent material.
Summary of the invention
The present invention has proposed a kind of novel preparation method of SiBON material on the basis for the SiBON investigation of materials.Control reaction process by controlling tetraethoxy and the consumption of boric acid, the addition of metallic silicon power and temperature and the soaking time of pressureless sintering, obtain the SiBON powder body material, then adopt dry pressing to obtain the SiBON base substrate, and carry out high-temperature calcination under nitrogen atmosphere, prepare the SiBON electromagnetic wave transparent material.The present invention has the advantages such as product purity is high, dielectric properties are excellent, stable mechanical property, in the aerospace cause electromagnetic wave transparent material such as radome in be widely used.
The novel preparation method of a kind of SiBON material that the present invention proposes.It is characterized in that: take tetraethoxy, boric acid, metallic silicon power as raw material, tetraethoxy is slowly dropped in boric acid solution, the water-bath magnetic agitation settles into gel after being added dropwise to complete.Dry in 120 ℃ of thermostatic drying chambers, with xerogel and metallic silicon power prepare burden, ball milling, dry pressuring forming process prepare base substrate, at N
2Under atmosphere, be incubated 2h-6h at the temperature of 1100 ℃-1500 ℃, being cooled to is to take out after room temperature to grind and cross 200 mesh sieves, obtains the SiBON powder.Powder is dry-pressing formed, and forming pressure is 5MPa-30MPa, and isostatic cool pressing pressure is 150MPa-200MPa, and the dwell time is 10s-90s.Base substrate is put into the atmosphere furnace of nitrogen protection, heat-up rate is 5 ℃/min, after insulation 1h-10h at 1400 ℃ of-1700 ℃ of temperature, can obtain the SiBON material after naturally cooling to room temperature.
The present invention propose a kind of high temperature solid-state method prepare the method for SiBON material, described technical process is specially:
1) tetraethoxy is slowly dropped in the boric acid solution of 1%-4.5%, use sodium dodecylbenzenesulfonate to make tensio-active agent, stir standing plastic under 80 ℃ of water-bath environment.Gel is placed in 120 ℃ of thermostatic drying chambers dry, it is stand-by that xerogel is levigate.
2) use 10 μ m～45 μ m metallic silicon powers and above-mentioned xerogel to prepare burden in the chemical equation ratio, dry grind in the planetary ball mill of packing into, particle diameter 1h-24h is uniformly dispersed to raw material.
3) raw material is dry-pressing formed, base substrate is put into the atmosphere furnace of nitrogen protection, heat-up rate is 1～10 ℃/min, takes out after naturally cooling to room temperature after insulation 2h-6h under 1100 ℃～1500 ℃, grinds and cross 200 mesh sieves.
4) powder that obtains is dry-pressing formed, pressure is 5MPa-30MPa, and the dwell time is 60s.Again sample is carried out isostatic cool pressing, pressure is 150MPa-200MPa, and the dwell time is 60s.
5) base substrate is put into the atmosphere furnace of nitrogen protection, heat-up rate is 5 ℃/min, and sintering at 1400 ℃ of-1700 ℃ of temperature, and insulation 1h-10h can obtain the SiBON material after naturally cooling to room temperature.
The present invention proposes a kind of method that pressureless sintering prepares the SiBON material.Control reaction process by controlling tetraethoxy and the consumption of boric acid, the addition of metallic silicon power and temperature and the soaking time of pressureless sintering, can obtain that purity is high, dielectric properties are excellent, the SiBON material of stable mechanical property, can be applied to the electromagnetic wave transparent material such as radome in, promote the development of aerospace cause.
Embodiment
Embodiment 1:
Material composition and granularity requirements that high temperature prepares the SiBON electromagnetic wave transparent material are: tetraethoxy, the massfraction of silicon-dioxide are 48.0%-50.0%; Boric acid, analytical pure; Deionized water; Metallic silicon power, 45 μ n; High pure nitrogen.
, tetraethoxy is slowly dropped in 3% boric acid solution than calculating the tetraethoxy add-on according to Si-B, use sodium dodecylbenzenesulfonate to make tensio-active agent, 80 ℃ of water-bath magnetic agitation, be added dropwise to complete rear standing plastic.Gel is placed in 120 ℃ of dryings of thermostatic drying chamber.After xerogel is levigate with 45 μ m metallic silicon powers by both certainty ratio batchings, in the planetary ball mill of packing into, dry grinding 12h is uniformly dispersed to raw material.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection, heat-up rate is 5 ℃/min, naturally cooling to room temperature after insulation 6h under 1100 ℃, grinds and cross 200 mesh sieves, obtains the SiBON powder body material.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carry out isostatic cool pressing, and pressure is 200MPa, the dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, and heat-up rate is 5 ℃/min, is incubated 6h under 1500 ℃, takes out after naturally cooling and obtains the SiBON material.
By the SiBON material that above-described embodiment 1 prepares, its strength at normal temperature value is 180MPa, and specific inductivity is 3.2.
Embodiment 2:
Material composition and granularity requirements that high temperature prepares the SiBON electromagnetic wave transparent material are: tetraethoxy, the massfraction of silicon-dioxide are 48.0%-50.0%; Boric acid, analytical pure; Deionized water; Metallic silicon power, 45 μ m; High pure nitrogen.
, tetraethoxy is slowly dropped in 3% boric acid solution than calculating the tetraethoxy add-on according to Si-B, use sodium dodecylbenzenesulfonate to make tensio-active agent, 80 ℃ of water-bath magnetic agitation, be added dropwise to complete rear standing plastic.Gel is placed in 120 ℃ of dryings of thermostatic drying chamber.After xerogel is levigate with 45 μ m metallic silicon powers by both certainty ratio batchings, in the planetary ball mill of packing into, dry grinding 12h is uniformly dispersed to raw material.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection, heat-up rate is 5 ℃/min, naturally cooling to room temperature after insulation 6h under 1200 ℃, grinds and cross 200 mesh sieves, obtains the SiBON powder body material.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carry out isostatic cool pressing, and pressure is 200MPa, the dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, and heat-up rate is 5 ℃/min, is incubated 6h under 1500 ℃, takes out after naturally cooling and obtains the SiBON material.
By the SiBON material that above-described embodiment 2 prepares, its strength at normal temperature value is 187MPa, and specific inductivity is 3.3.
Embodiment 3:
Material composition and granularity requirements that high temperature prepares the SiBON electromagnetic wave transparent material are: tetraethoxy, the massfraction of silicon-dioxide are 48.0%-50.0%; Boric acid, analytical pure; Deionized water; Metallic silicon power, 45 μ m; High pure nitrogen.
, tetraethoxy is slowly dropped in 3% boric acid solution than calculating the tetraethoxy add-on according to Si-B, use sodium dodecylbenzenesulfonate to make tensio-active agent, 80 ℃ of water-bath magnetic agitation, be added dropwise to complete rear standing plastic.Gel is placed in 120 ℃ of dryings of thermostatic drying chamber.After xerogel is levigate with 45 μ m metallic silicon powers by both certainty ratio batchings, in the planetary ball mill of packing into, dry grinding 12h is uniformly dispersed to raw material.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection, heat-up rate is 5 ℃/min, naturally cooling to room temperature after insulation 6h under 1300 ℃, grinds and cross 200 mesh sieves, obtains the SiBON powder body material.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carry out isostatic cool pressing, and pressure is 200MPa, the dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, and heat-up rate is 5 ℃/min, is incubated 6h under 1500 ℃, takes out after naturally cooling and obtains the SiBON material.
By the SiBON material that above-described embodiment 3 prepares, its strength at normal temperature value is 197MPa, and specific inductivity is 3.1.
Embodiment 4:
Material composition and granularity requirements that high temperature prepares the SiBON electromagnetic wave transparent material are: tetraethoxy, the massfraction of silicon-dioxide are 48.0%-50.0%; Boric acid, analytical pure; Deionized water; Metallic silicon power, 45 μ m; High pure nitrogen.
, tetraethoxy is slowly dropped in 3% boric acid solution than calculating the tetraethoxy add-on according to Si-B, use sodium dodecylbenzenesulfonate to make tensio-active agent, 80 ℃ of water-bath magnetic agitation, be added dropwise to complete rear standing plastic.Gel is placed in 120 ℃ of dryings of thermostatic drying chamber.After xerogel is levigate with 45 μ m metallic silicon powers by both certainty ratio batchings, in the planetary ball mill of packing into, dry grinding 12h is uniformly dispersed to raw material.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection, heat-up rate is 5 ℃/min, naturally cooling to room temperature after insulation 6h under 1400 ℃, grinds and cross 200 mesh sieves, obtains the SiBON powder body material.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carry out isostatic cool pressing, and pressure is 200MPa, the dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, and heat-up rate is 5 ℃/min, is incubated 6h under 1500 ℃, takes out after naturally cooling and obtains the SiBON material.
By the SiBON material that above-described embodiment 4 prepares, its strength at normal temperature value is 192MPa, and specific inductivity is 3.1.
Embodiment 5:
Material composition and granularity requirements that high temperature prepares the SiBON electromagnetic wave transparent material are: tetraethoxy, the massfraction of silicon-dioxide are 48.0%-50.0%; Boric acid, analytical pure; Deionized water; Metallic silicon power, 45 μ m; High pure nitrogen.
, tetraethoxy is slowly dropped in 3% boric acid solution than calculating the tetraethoxy add-on according to Si-B, use sodium dodecylbenzenesulfonate to make tensio-active agent, 80 ℃ of water-bath magnetic agitation, be added dropwise to complete rear standing plastic.Gel is placed in 120 ℃ of dryings of thermostatic drying chamber.After xerogel is levigate with 45 μ m metallic silicon powers by both certainty ratio batchings, in the planetary ball mill of packing into, dry grinding 12h is uniformly dispersed to raw material.Raw material is dry-pressing formed, sample is put into the atmosphere furnace of nitrogen atmosphere protection, heat-up rate is 5 ℃/min, naturally cooling to room temperature after insulation 6h under 1500 ℃, grinds and cross 200 mesh sieves, obtains the SiBON powder body material.Powder is dry-pressing formed, and pressure is 30MPa, pressurize 60s, then carry out isostatic cool pressing, and pressure is 200MPa, the dwell time is that 60s obtains ceramic body.Base substrate is put into atmosphere furnace, and heat-up rate is 5 ℃/min, is incubated 6h under 1500 ℃, takes out after naturally cooling and obtains the SiBON material.
By the SiBON material that above-described embodiment 5 prepares, its strength at normal temperature value is 198MPa, and specific inductivity is 2.9.
Claims (6)
1. a pressureless sintering prepares the method for SiBON material.It is characterized in that: take tetraethoxy, boric acid, metallic silicon power as raw material, tetraethoxy is slowly dropped in boric acid solution, stir standing plastic under the water-bath environment.Gel is placed in 120 ℃ of thermostatic drying chambers dry, after xerogel is levigate and metallic silicon power is prepared burden, ball milling, dry pressuring forming process prepare base substrate, at N
2Lower 1100 ℃ of-1500 ℃ of calcinings of atmosphere, insulation 2h-6h.Take out after naturally cooling, grind and cross 200 mesh sieves and obtain the SiBON powder body material.Powder is dry-pressing formed, make the atmosphere furnace that base substrate is put into the nitrogen atmosphere protection, heat-up rate is 5 ℃/min, naturally cools to room temperature and can obtain the SiBON material after insulation 1h-10h under 1400 ℃-1700 ℃.
2. preparation method according to claim 1 is characterized in that: the raw material of preparation SiBON electromagnetic wave transparent material is: tetraethoxy, the massfraction of silicon-dioxide are 48.0%-50.0%; Boric acid, analytical pure (99.99%); Deionized water; Metallic silicon power, 45 μ m; High pure nitrogen.
3. preparation method according to claim 1, it is characterized in that: the calcining temperature of SiBON powder body material is 1100 ℃-1500 ℃, insulation 2h-6h.
4. preparation method according to claim 1 is characterized in that: adopt dry pressing to obtain the SiBON base substrate, wherein dry-pressing formed pressure is 5MPa-30MPa, and the dwell time is 60s, and isostatic cool pressing pressure is 150MPa-200MPa, and the dwell time is 60s.
5. preparation method according to claim 1, it is characterized in that: the sintering temperature of SiBON stupalith is 1400 ℃-1700 ℃, and soaking time is 1h-10h.
6. preparation method according to claim 1, it is characterized in that: under described nitrogen atmosphere, the dividing potential drop of nitrogen is 0.01MPa-1.0MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106337217A (en) * | 2016-10-12 | 2017-01-18 | 中国人民解放军国防科学技术大学 | Porous Si-B-N-O ultra-fine fiber preparation method |
| CN114907128A (en) * | 2022-06-24 | 2022-08-16 | 中国人民解放军国防科技大学 | SiBNO heat-insulation wave-transparent integrated fiber and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6356464A (en) * | 1986-08-27 | 1988-03-11 | Tdk Corp | Thermal head |
| CN101104518A (en) * | 2007-08-24 | 2008-01-16 | 哈尔滨工业大学 | Process for preparing nano SiBON ceramic powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6356464A (en) * | 1986-08-27 | 1988-03-11 | Tdk Corp | Thermal head |
| CN101104518A (en) * | 2007-08-24 | 2008-01-16 | 哈尔滨工业大学 | Process for preparing nano SiBON ceramic powder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106337217A (en) * | 2016-10-12 | 2017-01-18 | 中国人民解放军国防科学技术大学 | Porous Si-B-N-O ultra-fine fiber preparation method |
| CN106337217B (en) * | 2016-10-12 | 2018-12-28 | 中国人民解放军国防科学技术大学 | A kind of porous Si-B-N-O superfine fibre and preparation method thereof |
| CN114907128A (en) * | 2022-06-24 | 2022-08-16 | 中国人民解放军国防科技大学 | SiBNO heat-insulation wave-transparent integrated fiber and preparation method and application thereof |
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