CN103341343B - A kind of preparation method of microwave synthetizing nano material heating container special - Google Patents
A kind of preparation method of microwave synthetizing nano material heating container special Download PDFInfo
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Abstract
The invention discloses heating container special of a kind of microwave synthetizing nano material and preparation method thereof, this container comprises vessel and container cover, and by the composite porous preparation of ceramic alumina fiber.Selective oxidation aluminium ceramic fibre of the present invention is composite porous (mainly containing Al
2o
3) replace traditional common refractory, can cushion the container thermal expansion stress because pyroreaction material causes, improve the thermal shock resistance that heating container material in microwave field is rapidly heated, not easily burst, material use ceramic fibre strengthens toughness.Significantly improve microwave transparent rate, high insulating effect by selecting the material of suitable low dielectric loss and reducing the configuration design of stress, and preparation technology is simple, cost is low and can carry out large-scale industrial production.
Description
Technical field
The present invention relates to nano material synthesis technical field, be specifically related to heating container special being applicable to adopt microwave heating nano materials and preparation method thereof.
Background technology
Nano material, as a focus of investigation of materials, fundamentally changes the structure of material.Nano material refers to and is made up of fines, and characteristic dimension size is at the material of nanometer scale (1 ~ 100nm).Due to superfine crystal grain and the atom that is in a large number in crystal boundary and crystal grain in defect, nano material has the difference of highly significant with the material with the micron order that forms or more in performance, can produce important impact to the electricity of material, calorifics, magnetics, optical characteristics.Therefore, the progress of research to modern science and technology of nano materials has great meaning.
Just gradually upsurge has been risen since utilizing microwave synthetizing nano material technology to be the eighties in 20th century, this synthetic technology saves time, energy-conservation and firing rate can up to 500 DEG C/min, crystal grain can being made to complete synthesis when having little time to grow up, forming evenly neat grainiess.Microwave synthesize has larger advantage than conventional nano materials powder: (1) synthesis temperature obviously reduces.Because rate of warming is fast, decrease hot loss of energy.(2) generated time is short.Save mass energy.Become today of the common issue of facing mankind in energy-conserving and environment-protective, utilize microwave synthetizing nano material technology can economize energy improve efficiency of energy utilization, significant to the sustainable development of China.
At present, in this area domestic and international microwave synthetizing nano material heating container prepare the conventional refractory material containers of multiselect.In microwave synthetizing nano materials process, nano material is loaded in heating container, then nano material is put in microwave field together with heating container and heat.So the performance requirement of heating container in microwave field is harsh especially, it is also one of key technical problem of microwave synthetizing nano Material Field.
Tradition refractory material heating container finds that in microwave field there are the following problems: (1) container easily bursts.Heating using microwave speed and rate of rise in temperature are very fast, and container contents irregularly very easily causes synthesis temperature just and synthetic ratio is different more easily bursts because being heated.(2) container own material meeting microwave energy absorbing, container self-temperature is made to increase very fast, not only increase the possibility of container ruptures, and it is very high to make container outer surface temperature increase, make in microwave burner hearth and intra passage temperature uprises, increase difficulty and the process dangerous of microwave burner hearth Material selec-tion.(3) heat temperature raising is uneven.Due to container material quality inhale ripple make microwave transparent uneven, cause the inequality of being heated at each position of nanomaterial building-up process, nano materials very easily reunite or synthetic ratio not high, crystal grain easily produces defect.(4) heat insulating ability is bad.Cannot be at high temperature material insulation, for the nanomaterial requiring to react at a certain temperature, traditional refractory material containers pole be not suitable for, and cannot keep even and stable temperature.
Summary of the invention
The defect that the present invention exists to overcome existing nano materials heating container technology, provides one both easy wave transparents, can play again the durable and efficient microwave synthetizing nano heating materials container of insulation effect.Design alternative main purpose be a kind of can wave transparent, do not inhale ripple, can be incubated and have the container of some strength to be the key of dealing with problems.The invention solves the easily explosion in microwave field of conventional heating container, synthesized material is heated, and grain crystalline degree that is uneven, nano materials is bad, synthetic ratio is not high or easily reunite, heat insulation effect is bad makes container outer wall temperature high-technology problem.
For overcoming the above problems, technical scheme of the present invention is as follows:
A heating container special for microwave synthetizing nano material, this container comprises vessel and container cover, and by the composite porous preparation of ceramic alumina fiber.
Preferably, described container is column type.
Preferably, the high 23 ~ 25cm of described container, wall thickness 3.5cm, bottom surface inner circle radius 8cm, the thick 3cm of container cover, base thickness 3cm.
Preferably, described container cover is provided with thermometer hole.
Preferably, the aperture of described thermometer hole is 1.0cm.
The preparation method of above-mentioned heating container, comprises the steps:
(1) soak in composite porous for ceramic alumina fiber immersion distilled water, after complete wetting, with colloid mill, fiber is pulverized, make single fiber maximum length be no more than 5mm;
(2) distilled water is mixed by 1:1 volume ratio with alcohols solvent, then by water 500ml, add 2 ~ 5ml hydrochloric acid, slowly ethyl orthosilicate is added again with buret, constantly stir simultaneously, the weight ratio of described ethyl orthosilicate and alcohols solvent was 1:1, by still aging 2 hours of the teos hydrolysis liquid for preparing;
(3) above-mentioned teos hydrolysis liquid is mixed with ceramic alumina fiber is composite porous, put into mould compressing;
(4) will suppress ceramic fiber body and leave standstill 2 ~ 3 hours, then form removal, puts into oven for drying;
(5) base substrate of oven dry is put into stove and rise to 1200 DEG C with 4 DEG C/min heating rate, be incubated one hour, cool in stove.
Preferably, step (2) described alcohols solvent is ethanol or isopropyl alcohol.
Preferably, the described teos hydrolysis liquid of step (3) and Al
3o
2the weight ratio of ceramic fibre mixing is 1:(3 ~ 3.5).
Preferably, step (3) described briquetting pressure is 50kg/cm
2.
Each performance data of obtained heating container special is as follows:
Most high-temperature resistant: 2000 DEG C, thermal conductivity factor: 0.017W/m.k, compression strength: 4.5 ~ 5.2Mpa, rupture strength 1.3 ~ 2Mpa, linear expansion coefficient: 1.6 × 10
-7mm/ DEG C, porosity is 85%-96%.
Compared with traditional refractory material heating container, the present invention has following beneficial effect:
(1) selective oxidation aluminium ceramic fibre of the present invention is composite porous (mainly containing Al
2o
3) replace traditional common refractory, due to Al
2o
3do not inhale ripple and improve the penetrance of microwave, and its porous energy, the container thermal expansion stress that pyroreaction material causes can be cushioned, the composite porous thermal shock resistance that can improve heating container of Material selec-tion, avoid container easily to break at rapid heating condition, can also insulation effect be played.Do not absorb microwave due to this material and can greatly improve microwave transparent rate, microwave transparent rate is increased to 99% by original 80%.
(2) inventive container lid center drilling is beneficial to thermometric, and gets rid of in time the excess air that produces in synthesis to keep stablizing of temperature and pressure in container, prevents container from ftractureing.The wall thickness of design heating container is 3.5 centimetres, is conducive to being incubated and ensureing the even of temperature in casket Bowls, can avoid the generation of container temperature difference in nano material synthetic reaction process, and too fast temperature rise causes the Decrepitation Phenomena of Bowls body.Preparation method of the present invention is simple, and highly effective, product is easy to industrialization.
(3) the present invention adopts ceramic alumina fiber composite porous, enhances the intensity (compression strength: 4.5 ~ 5.2Mpa, rupture strength: 1.3 ~ 2Mpa) of container.Design employs the cylindrical shape not easily producing stress, and the Volume Changes that material causes because of variations in temperature is very little, and the stress of generation is little, makes container more highly efficient durable (most high-temperature resistant: 2000 DEG C), not easily bursts at rapid heating condition.
(4) relative to porous material, the structure of heating container of the present invention is closed cylindrical type, the design of the height of its cylinder, end radius of circle and thickness relates to heat trnasfer gradient problem, thus can ensure its good in insulation effect, enhances the heat insulation effect of container.In addition, heating container structure of the present invention due to porous and use ceramic fibre make nano materials also enhance its heat insulation effect.Even if reaction mass reaction temperature reaches more than 1300 DEG C, the microwave burner hearth cavity temperature outside container is only about 50 DEG C, and heat insulation effect is very good, greatly reduces the requirement of burner hearth material to heat resistance.Therefore the general stainless steel of design microwave burner hearth just can be competent at, and has both reduced microwave industrial furnace materials cost, the outer industrial site environmental amenity of stove and safety can be protected again.
Accompanying drawing explanation
Fig. 1 is the structural representation of the heating container of microwave synthetizing nano material of the present invention.
Fig. 2 is heating container environment for use schematic diagram of the present invention, 1, heating container, 2, magnetron, 3, mica delivery board, 4, optics thermal detector, 5, high-temperature nano material.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is more specifically described in detail, but embodiments of the present invention are not limited thereto, for the technological parameter do not indicated especially, can refer to routine techniques and carry out.
Embodiment 1
The preparation method of the heating container special of microwave synthetizing nano material, comprises the steps:
1, composite porous for ceramic alumina fiber (being purchased from the Sanmenxia Gorge, Henan Xi Hongtai Lu Ye Technology Co., Ltd.) is immersed in distilled water and soaked, after complete wetting, with colloid mill, fiber is pulverized, make single fiber maximum length be no more than 5mm.
2, distilled water is mixed by 1:1 volume ratio with ethanol, then 4ml hydrochloric acid (by water 500ml) is added, then slowly ethyl orthosilicate is added with buret, constantly stir simultaneously, the weight ratio of ethyl orthosilicate and ethanol was 1:1, by still aging 2 hours of the teos hydrolysis liquid for preparing.
3, composite porous with ceramic alumina fiber for above-mentioned teos hydrolysis liquid (1:3 weight ratio) mixed, put into mould compressing, briquetting pressure is 50kg/cm
2.
4, will suppress ceramic fiber body and leave standstill 2 hours, then form removal, puts into oven for drying.
5, the base substrate of oven dry is put into stove and rise to 1200 DEG C with 4 DEG C/min heating rate, be incubated 1 hour, cool in stove, can use.
Heating container 1 prepared by said method comprises vessel 11 and container cover 12, and container cover 12 center is provided with diameter 1cm thermometer hole 13, in infrared measurement of temperature instrument test container in microwave field, synthesis temperature provides passage.Container height overall 25cm, wall thickness 3.5cm, bottom surface inner circle radius 8cm, container base thickness 3cm, the thick 3cm of container cover.
The performance of described microwave synthetizing nano material heating container special is as follows:
Most high-temperature resistant: 2000 DEG C, thermal conductivity factor: 0.017W/m.k, thermal coefficient of expansion is 1.6 × 10
-7mm/ DEG C, compression strength: 5Mpa, rupture strength: 2Mpa.Porosity is 85%-93%, bulk density 0.7g/cm
3, weight is 0.5Kg.
Embodiment 2
The difference of the present embodiment and embodiment 1 is only:
Utilize long chain alkanol (isopropyl alcohol) to replace ethanol to prepare ethyl orthosilicate precursor (teos hydrolysis liquid), obtained heating container performance is as follows:
Most high-temperature resistant: 2000 DEG C, thermal conductivity factor: 0.017W/m.k, thermal coefficient of expansion is 1.6 × 10
-7mm/ DEG C, compression strength: 5.2Mpa, rupture strength: 1.7Mpa.Porosity is 86%-94%, bulk density 0.6g/cm
3, weight is 0.48Kg.
Embodiment 3
The difference of the present embodiment and embodiment 1 is only:
Ethyl orthosilicate precursor and the composite porous weight ratio of ceramic alumina fiber of preparation are 1:3.5, and obtained heating container performance is as follows:
Most high-temperature resistant: 2000 DEG C, thermal conductivity factor: 0.017W/m.k, thermal coefficient of expansion is 1.6 × 10
-7mm/ DEG C, compression strength: 4.5Mpa, rupture strength: 1.3Mpa.Porosity is 88%-96%, bulk density 0.7g/cm
3, weight is 0.53Kg.
In sum, the present invention improves the thermal shock resistance that heating container material in microwave field is rapidly heated, and not easily bursts, and material use ceramic fibre strengthens toughness.Significantly improve microwave transparent rate, high insulating effect by selecting the material of suitable low dielectric loss and reducing the configuration design of stress, and preparation technology is simple, cost is low and can carry out large-scale industrial production.
Claims (4)
1. a preparation method for microwave synthetizing nano material heating container special, is characterized in that, this container comprises vessel and container cover, and by the composite porous preparation of ceramic alumina fiber, preparation method comprises the steps:
(1) soak in composite porous for ceramic alumina fiber immersion distilled water, after complete wetting, with colloid mill, fiber is pulverized, make single fiber maximum length be no more than 5mm;
(2) distilled water is mixed by 1:1 volume ratio with alcohols solvent, then by water 500 mL, add 2 ~ 5 mL hydrochloric acid, slowly ethyl orthosilicate is added again with buret, constantly stir simultaneously, the weight ratio of described ethyl orthosilicate and alcohols solvent was 1:1, by still aging 2 hours of the teos hydrolysis liquid for preparing;
(3) above-mentioned teos hydrolysis liquid is mixed with ceramic alumina fiber is composite porous, put into mould compressing;
(4) will suppress ceramic fiber body and leave standstill 2 ~ 3 hours, then form removal, puts into oven for drying;
(5) base substrate of oven dry is put into stove and rise to 1200 DEG C with 4 DEG C/min heating rate, be incubated 1 hour, cool in stove.
2. preparation method according to claim 1, is characterized in that, step (2) described alcohols solvent is ethanol or isopropyl alcohol.
3. preparation method according to claim 1 and 2, is characterized in that, step (3) described teos hydrolysis liquid is 1:(3 ~ 3.5 with the composite porous weight ratio mixed of ceramic alumina fiber).
4. preparation method according to claim 1 and 2, is characterized in that, step (3) described briquetting pressure is 50kg/cm
2.
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| CN103816850A (en) * | 2014-01-16 | 2014-05-28 | 南昌大学 | Microwave output energy controllable pyrolysis method and device of unit mass reactors |
| CN112794725A (en) * | 2021-03-17 | 2021-05-14 | 中钢南京环境工程技术研究院有限公司 | Preparation method of alumina fiber lining material for industrial microwave kiln |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686945A (en) * | 2005-04-01 | 2005-10-26 | 清华大学 | Silica sol solidification method for forming ceramic component |
| CN1694584A (en) * | 2005-05-27 | 2005-11-09 | 张敬胜 | Microwave heating apparatus |
| CN101568208A (en) * | 2009-01-21 | 2009-10-28 | 徐艳姬 | Microwave and heating element combined heating type heating chamber and manufacturing method thereof |
| CN101948325A (en) * | 2010-09-14 | 2011-01-19 | 浙江科技学院 | Synergistic toughening alumina ceramic and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1686945A (en) * | 2005-04-01 | 2005-10-26 | 清华大学 | Silica sol solidification method for forming ceramic component |
| CN1694584A (en) * | 2005-05-27 | 2005-11-09 | 张敬胜 | Microwave heating apparatus |
| CN101568208A (en) * | 2009-01-21 | 2009-10-28 | 徐艳姬 | Microwave and heating element combined heating type heating chamber and manufacturing method thereof |
| CN101948325A (en) * | 2010-09-14 | 2011-01-19 | 浙江科技学院 | Synergistic toughening alumina ceramic and preparation method thereof |
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