CN103341343A - Dedicated heating container for microwave synthesis of nanomaterials and preparation method thereof - Google Patents
Dedicated heating container for microwave synthesis of nanomaterials and preparation method thereof Download PDFInfo
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- CN103341343A CN103341343A CN2013102224483A CN201310222448A CN103341343A CN 103341343 A CN103341343 A CN 103341343A CN 2013102224483 A CN2013102224483 A CN 2013102224483A CN 201310222448 A CN201310222448 A CN 201310222448A CN 103341343 A CN103341343 A CN 103341343A
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Abstract
The invention discloses a dedicated heating container for microwave synthesis of nanomaterials and a preparation method thereof. The container comprises a container body and a container cover which are both made of an alumina ceramic fiber porous composite material. The alumina ceramic fiber porous composite material (mainly containing Al2O3) is selected for replacing a conventional common refractory material, and thus a container thermal expansion stress caused by a high temperature reaction material is buffered, a thermal shock resistance property of the heating container is promoted when the material is rapidly heated up in a microwave field, the heating container is not easy to crack, and a ceramic fiber is utilized to reinforce toughness in the material. With selection of a suitable material with low dielectric loss and a shape design capable of reducing stress, the microwave transmittance is significantly improved, and the heat insulation effect is good; and the preparation method has simple preparation process, is low in cost, and can be applied to large-scale industrial production.
Description
Technical field
The present invention relates to the nano material synthesis technical field, be specifically related to be applicable to special-purpose heating container that adopts the microwave heating nano materials and preparation method thereof.
Background technology
Nano material has fundamentally changed the structure of material as a focus of investigation of materials.Nano material refers to be made up of fines, and the characteristic dimension size is at nanometer scale (1～100nm) material.Because superfine crystal grain and be in crystal boundary in a large number and the intragranular defective in atom, nano material on performance with the difference that highly significant is arranged with the micron order of forming or above material, can produce significant effects to electricity, calorifics, magnetics, the optical characteristics of material.Therefore, the research of nano materials has significant meaning to the progress of modern science and technology.
Utilizing the microwave synthetizing nano material technology is just to have risen upsurge gradually since the eighties in 20th century, this synthetic technology saves time, energy-conservation and firing rate can be up to 500 ℃/min, can make crystal grain under the situation that has little time to grow up and finish syntheticly, form evenly neat grainiess.Microwave is synthetic to have bigger advantage than conventional nano materials powder: (1) synthesis temperature obviously reduces.Because rate of warming is fast, reduced the loss of heat energy.(2) generated time is short.A large amount of energy have been saved.Become today of common problem human being face in energy-conserving and environment-protective, utilized the microwave synthetizing nano material technology can energy savings and improve efficiency of energy utilization, significant to the sustainable development of China.
At present, the conventional refractory material container of the preparation multiselect of domestic and international microwave synthetizing nano material heating container in this area.In the microwave synthetizing nano materials process, nano material is packed in the heating container, nano material and heating container are put in the microwave field together heated then.So the performance requirement of heating container in microwave field is harsh especially, also is one of the key technical problem in microwave synthetizing nano material field.
Tradition refractory material heating container finds that in microwave field there are the following problems: the easy explosion of (1) container.Heating using microwave speed and rate of rise in temperature are very fast, and material is because of irregular very easily cause synthesis temperature height and the different easier generation explosion of synthetic ratio of being heated in the container.(2) material of container own can absorb microwave energy, it is very fast that the container self-temperature is risen, and not only increases the possibility of container explosion, and it is very high that the container outer surface temperature is risen, the interior interior temperature of passage that reaches of microwave burner hearth is uprised, increase difficulty and technology danger that microwave burner hearth material is selected.(3) heat temperature raising is inhomogeneous.Make microwave penetrating inhomogeneous because the container material is inhaled ripple, 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 defective.(4) heat insulating ability is bad.Can't at high temperature be the material insulation, for the nanomaterial that requires to react at a certain temperature, traditional refractory material container utmost point is not suitable for, and can't keep even and stable temperature.
Summary of the invention
The present invention provides a kind of both easily saturating ripple in order to overcome the defective that existing nano materials heating container technology exists, and can play the durable and efficient microwave synthetizing nano material heating container of insulation effect again.The design alternative main purpose is a kind of ripple thoroughly, not inhale ripple, can be incubated and have the container of certain intensity be the key of dealing with problems.The invention solves the easily explosion in microwave field of conventional heating container, bad, the not high or easy reunion of synthetic ratio of crystal grain degree of crystallinity inhomogeneous, nano materials of being heated of synthetic material, the bad container outer wall temperature high-technology problem that makes of heat insulation effect.
For overcoming the above problems, technical scheme of the present invention is as follows:
A kind of special-purpose heating container of 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, radius of circle 8cm in the bottom surface, 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) with soaking in the composite porous immersion distilled water of ceramic alumina fiber, after the complete wetting, with colloid mill fiber is pulverized, made single fiber maximum length be no more than 5mm;
(2) distilled water is mixed by the 1:1 volume ratio with alcohols solvent, then by water 500ml, add 2～5ml hydrochloric acid, slowly add ethyl orthosilicate with buret again, constantly stir simultaneously, the weight ratio of described ethyl orthosilicate and alcohols solvent was 1:1, with still aging 2 hours of the teos hydrolysis liquid for preparing;
(3) with above-mentioned teos hydrolysis liquid and ceramic alumina fiber is composite porous mixes, put into mould compression moulding;
(4) will suppress the ceramic fibre base substrate and leave standstill 2～3 hours, oven for drying is put in form removal then;
(5) base substrate of oven dry is put into stove and risen to 1200 ℃ with 4 ℃/min heating rate, be incubated one hour, in stove, cool off and get final product.
Preferably, the described alcohols solvent of step (2) is ethanol or isopropyl alcohol.
Preferably, the described teos hydrolysis liquid of step (3) and Al
3O
2The weight ratio that ceramic fibre mixes is 1:(3～3.5).
Preferably, the described briquetting pressure of step (3) is 50kg/cm
2
Each performance data of the special-purpose heating container that makes is as follows:
High-temperature resistant: 2000 ℃, 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/ ℃, porosity is 85%-96%.
Compare 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 contains Al
2O
3) replace traditional common refractory, because Al
2O
3Do not inhale ripple and improve the penetrance of microwave, with and the porous energy, can cushion the container thermal expansion stress that the pyroreaction material causes, material is selected the composite porous thermal shock resistance that can improve heating container, avoid container easily to break in the process of being rapidly heated, can also play insulation effect.Because this material does not absorb microwave and can not improve the microwave penetrating rate greatly, the microwave penetrating rate is increased to 99% by original 80%.
(2) container cover center drilling of the present invention is beneficial to thermometric, and in time gets rid of the excess air that produces in synthetic to keep the stable of temperature and pressure in the container, prevents the container cracking.The wall thickness of design heating container is 3.5 centimetres, is conducive to be incubated and guarantee the even of the interior temperature of casket Bowls, can avoid the generation of container temperature difference in the nano material synthetic reaction process, and too fast temperature rise causes the explosion phenomenon of Bowls body.Preparation method of the present invention is simple, highly effective, and product is easy to industrialization.
(3) the present invention adopts ceramic alumina fiber composite porous, has strengthened intensity (compression strength: 4.5～5.2Mpa, the rupture strength: 1.3～2Mpa) of container.The cylindrical shape of difficult generation stress has been used in design, and material is very little because of the Volume Changes that variations in temperature causes, the stress of generation is little, makes more highly efficient durable (high-temperature resistant: 2000 ℃) of container, is difficult for explosion in the process of being rapidly heated.
(4) with respect to porous material, the structure of heating container of the present invention is closed cylindrical type, and the design of the height of its cylinder, end radius of circle and thickness relates to heat and transmits gradient problem, thereby can guarantee that its effect of heat insulation is good, has strengthened the heat insulation effect of container.In addition, heating container structure of the present invention is because porous and use ceramic fibre make nano materials also strengthen its heat insulation effect.Even the reaction mass reaction temperature reaches more than 1300 ℃, the outer microwave burner hearth cavity temperature of container only is that heat insulation effect is very good about 50 ℃, greatly reduces the burner hearth material to the requirement of heat resistance.So design microwave burner hearth just can be competent at general stainless steel, has both reduced microwave industrial furnace materials cost, can protect the outer industrial site environmental amenity of stove and safety again.
Description of drawings
Fig. 1 is the structural representation of microwave synthetizing nano material heating container of the present invention.
Fig. 2 is heating container environment for use schematic diagram of the present invention, 1, heating container, 2, magnetron, 3, the mica delivery board, 4, the optics thermal detector, 5, the high-temperature nano material.
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiments of the present invention are not limited thereto, the technological parameter for not indicating especially can carry out with reference to routine techniques.
Embodiment 1
The preparation method of the special-purpose heating container of microwave synthetizing nano material comprises the steps:
1, ceramic alumina fiber composite porous (purchasing in the Sanmenxia Gorge, Henan Xi Hongtai stove industry technology Co., Ltd) is immersed in the distilled water and soaks, after the complete wetting, with colloid mill fiber is pulverized, make single fiber maximum length be no more than 5mm.
2, distilled water is mixed by the 1:1 volume ratio with ethanol, add 4ml hydrochloric acid (by water 500ml) then, slowly add ethyl orthosilicate with buret then, constantly stir simultaneously, the weight ratio of ethyl orthosilicate and ethanol was 1:1, with still aging 2 hours of the teos hydrolysis liquid for preparing.
3, above-mentioned teos hydrolysis liquid and ceramic alumina fiber composite porous (1:3 weight ratio) are mixed, put into mould compression moulding, briquetting pressure is 50kg/cm
2
4, will suppress the ceramic fibre base substrate and leave standstill 2 hours, oven for drying is put in form removal then.
5, the base substrate of oven dry is put into stove and rise to 1200 ℃ with 4 ℃/min heating rate, be incubated 1 hour, in stove, cool off, can use.
The heating container 1 of method for preparing comprises vessel 11 and container cover 12, and container cover 12 centers are provided with diameter 1cm thermometer hole 13, for synthesis temperature in the infrared measurement of temperature instrument test container in the microwave field provides passage.Container height overall 25cm, wall thickness 3.5cm, radius of circle 8cm in the bottom surface, container base thickness 3cm, the thick 3cm of container cover.
The performance of the special-purpose heating container of described microwave synthetizing nano material is as follows:
High-temperature resistant: 2000 ℃, thermal conductivity factor: 0.017W/m.k, thermal coefficient of expansion are 1.6 * 10
-7Mm/ ℃, compression strength: 5Mpa, rupture strength: 2Mpa.Porosity is 85%-93%, bulk density 0.7g/cm
3, weight is 0.5Kg.
The difference of present embodiment and embodiment 1 only is:
Utilize long chain alkanol (isopropyl alcohol) to replace ethanol preparation ethyl orthosilicate precursor (teos hydrolysis liquid), it is as follows to make the heating container performance:
High-temperature resistant: 2000 ℃, thermal conductivity factor: 0.017W/m.k, thermal coefficient of expansion are 1.6 * 10
-7Mm/ ℃, 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 present embodiment and embodiment 1 only is:
Ethyl orthosilicate precursor and the composite porous weight ratio of ceramic alumina fiber of preparation are 1:3.5, and it is as follows to make the heating container performance:
High-temperature resistant: 2000 ℃, thermal conductivity factor: 0.017W/m.k, thermal coefficient of expansion are 1.6 * 10
-7Mm/ ℃, 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 has promoted the heating container thermal shock resistance that material is rapidly heated in microwave field, is difficult for explosion, and the material use ceramic fibre strengthens toughness.Significantly improve the microwave penetrating rate by the material of selecting suitable low dielectric loss and the configuration design that reduces stress, high insulating effect, and also preparation technology is simple, and cost is low and can carry out large-scale industrial production.
Claims (9)
1. the special-purpose heating container of a microwave synthetizing nano material is characterized in that, this container comprises vessel and container cover, and by the composite porous preparation of ceramic alumina fiber.
2. according to the described heating container of claim 1, it is characterized in that described container is column type.
3. according to claim 1 or 2 described heating containers, it is characterized in that described container height overall 23～25cm, wall thickness 3.5cm, radius of circle 8cm in the bottom surface, container base thickness 3cm, the thick 3cm of container cover.
4. according to the described heating container of claim 3, it is characterized in that described container cover is provided with thermometer hole.
5. according to the described heating container of claim 4, it is characterized in that the aperture of described thermometer hole is 1.0cm.
6. the preparation method of any described heating container of claim 1～5 is characterized in that, comprises the steps:
(1) with soaking in the composite porous immersion distilled water of ceramic alumina fiber, after the complete wetting, with colloid mill fiber is pulverized, made single fiber maximum length be no more than 5mm;
(2) distilled water is mixed by the 1:1 volume ratio with alcohols solvent, then by water 500ml, add 2～5ml hydrochloric acid, slowly add ethyl orthosilicate with buret again, constantly stir simultaneously, the weight ratio of described ethyl orthosilicate and alcohols solvent was 1:1, with still aging 2 hours of the teos hydrolysis liquid for preparing;
(3) with above-mentioned teos hydrolysis liquid and ceramic alumina fiber is composite porous mixes, put into mould compression moulding;
(4) will suppress the ceramic fibre base substrate and leave standstill 2～3 hours, oven for drying is put in form removal then;
(5) base substrate of oven dry is put into stove and risen to 1200 ℃ with 4 ℃/min heating rate, be incubated 1 hour, in stove, cool off and get final product.
7. preparation method according to claim 6 is characterized in that, the described alcohols solvent of step (2) is ethanol or isopropyl alcohol.
8. according to claim 6 or 7 described preparation methods, it is characterized in that the described teos hydrolysis liquid of step (3) is 1:(3～3.5 with the composite porous weight ratio of mixing of ceramic alumina fiber).
9. according to claim 6 or 7 described preparation methods, it is characterized in that the described briquetting pressure of step (3) is 50kg/cm
2
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2013
- 2013-06-06 CN CN201310222448.3A patent/CN103341343B/en active Active
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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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