CN106673671B - A kind of synchroballistic Microwave Hybrid co-sintering method - Google Patents
A kind of synchroballistic Microwave Hybrid co-sintering method Download PDFInfo
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- CN106673671B CN106673671B CN201710024851.3A CN201710024851A CN106673671B CN 106673671 B CN106673671 B CN 106673671B CN 201710024851 A CN201710024851 A CN 201710024851A CN 106673671 B CN106673671 B CN 106673671B
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Abstract
The invention discloses a kind of synchroballistic Microwave Hybrid co-sintering methods, belong to microwave sintering ceramic technical field.This method comprises the following steps: the high dielectric loss ceramic of low temperature and low temperature low dielectric loss ceramic are put into microwave resonance cavity jointly；Gradient adjusts microwave input power and elevates the temperature to 1350-1550 DEG C；Microwave input power is finely tuned, 30-50min is kept the temperature；Then power is downgraded into 1.5-2.5kW, temperature is made to be reduced to 750-850 DEG C, close microwave source, Temperature fall.The present invention utilizes the microwave coupling performance difference of different ceramics, realizes ceramic synchroballistic Microwave Hybrid co-sintering, can be improved the production efficiency of ceramic, moreover it is possible to improve capacity usage ratio.
Description
Technical field
The present invention relates to a kind of synchroballistic Microwave Hybrid co-sintering methods, belong to microwave sintering ceramic technology neck
Domain.
Background technique
Microwave heating energy saving, efficient, the free of contamination sintering technology emerging as one, is widely used to daily life
In.Ceramic body has to just make mutually to bond between particle by the sintering of high temperature, and being formed has some strength, hardness
Ceramic body.Existing sintering process mostly uses normal sintering, and there are the sintering period is long, production efficiency is low, sintering temperature is high and energy
The problem of source wastes.Microwave sintering is couple with material using special wave band possessed by microwave generating heat, and material is logical
The dielectric loss of itself is crossed to absorb electromagnetic energy and entirety is made to be heated to sintering temperature, there is entirety to heat, be evenly heated, selectivity
The features such as heating, be easy to control, is energy-efficient.
Currently, the ceramic material of microwave sintering mainly includes silicon carbide, and zirconium oxide, aluminium oxide, silicon nitride, titanium carbide etc.
Deng.Because the dielectric loss difference of various ceramic materials is larger, even if ceramic material of the same race is in different temperature ranges, medium
Loss also has very big difference.The difference of dielectric loss causes ceramic material to the difference of microwave absorbing property, so as to cause heating
The difference of effect.By taking zirconia ceramics as an example, since dielectric loss is lower under its room temperature, using the sintering side of auxiliary heating
Formula, first production auxiliary heating and thermal insulation structure generate heat using the good performance for absorbing microwave of auxiliary heating body room temperature,
To zirconia ceramics radiant heating, to 400 DEG C or so, zirconia media loss is increased, and realizes microwave heating.Same principle,
It during to complex phase ceramic sintering, is heated using the selectivity of microwave, high lossy medium absorbs microwave in complex phase ceramic, is formed
Internal heat resource eventually forms whole heating mode to heat low loss dielectric.The method can assist heating to avoid using
Body, but it is only limitted to the sintering of composite ceramic material.
Publication No. is that CN104326751A Chinese invention patent discloses a kind of ZTA ceramic microwave sintering method, this method
It has successfully been burnt into large-sized bias ZTA ceramic valve using microwave, has greatly reduced sintering time, while the localized heat proposed
Amount compensation principle also provides a kind of theoretical foundation for the irregular ceramic of microwave sintering.However, relevant in the prior art
Study limitation is in the microwave sintering of single ceramic material, i.e., in a microwave heating cycle, only for a kind of ceramic material into
Row microwave sintering.The microwave sintering method of this single ceramic, is bound to cause a large amount of energy waste.For conventional low damage
Ceramic is consumed, needs to add auxiliary heating body, low-loss ceramic 1 as shown in Figure 1 needs auxiliary heating body 2 to be assisted
Heat-agglomerating, this just indirectly increases the consumption of microwave energy；Correspondingly, the ceramic of room temperature height loss, it is micro- absorbing
During wave generates heat, the heat of its own radiation is not also utilized and consumes.Energy wave during this microwave sintering
It is badly in need of the problem of taking solving.
Summary of the invention
The object of the present invention is to provide a kind of synchroballistic Microwave Hybrid co-sintering method, during solving microwave sintering
The problem of energy waste, improves the efficiency of microwave sintering.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
A kind of synchroballistic Microwave Hybrid co-sintering method, includes the following steps:
1) the high dielectric loss ceramic of low temperature and low temperature low dielectric loss ceramic are put into microwave cavity jointly
In body；
2) microwave input power is adjusted to 1.5-2.5kW, when heating rate is lower than 2 DEG C/min, adjusts microwave input work
Rate adjusts input power to 5.5-6.5kW again, is warming up to 3.5-4.5kW when heating rate is again below 2 DEG C/min
1350-1550℃；
3) input power is finely tuned, it is made to keep the temperature 30-50min；
4) power is then downgraded into 1.5-2.5kW, temperature is made to be reduced to 750-850 DEG C, close microwave source, dropped naturally
Temperature.
When microwave input power being adjusted to 1.5-2.5kW in the step 2), heating rate is 2-20 DEG C/min.
When adjusting microwave input power in the step 2) to 3.5-4.5kW, heating rate is 2-15 DEG C/min.
Preferably, the high dielectric loss ceramic of the low temperature and low temperature low dielectric loss ceramic are put into guarantor jointly
In warm device, then attemperator is put into microwave resonance cavity.
The high dielectric loss ceramic of low temperature is silicon carbide ceramics.
The low temperature low dielectric loss ceramic is zirconia ceramics.
Preferably, the high dielectric loss ceramic of the low temperature is silicon carbide ceramic.
Preferably, the low temperature low dielectric loss ceramic is zirconia ceramics pipe, zirconia ceramics ring, zirconium oxide pottery
Tile.
It is further preferred that its consistency of the zirconia ceramics is splendid, apparent porosity 0.03%.
During synchroballistic Microwave Hybrid co-sintering of the invention, when microwave power is constant, heating rate can gradually become
Slowly, it is therefore desirable to which adjusting microwave input rate makes temperature rise to required temperature.Gradually slack-off reason is ceramic blank to heating rate
Organic matter binding agent couples strongly with microwave in cold stage in body, and sample is promoted to be rapidly heated before 300 DEG C.With organic
The exclusion of object, heating rate gradually slow down, but are not greatly lowered, the reason is that the silicon carbide system of the high dielectric loss of initial stage of sintering
Product absorb microwave, and self-heating radiations heat energy balances whole heating rate, after 800 DEG C, with the raising of input power,
Heating rate keeps balance, illustrates the enhancing with microwave coupling ability and silicon carbide and microwave coupling ability of zircite product
Decrease reaches relative equilibrium.
Synchroballistic Microwave Hybrid co-sintering method in the present invention, that is, utilize the ceramic of the high dielectric loss of low temperature processed
Good absorbing microwave capability absorbs microwave in cold stage, conducting self-heating sintering is realized, and can be used as heat source, to low temperature
The ceramic of low dielectric loss carries out radiant heating；When temperature is increased to high-temperature region, the product medium of low temperature low dielectric loss
Loss increases, and starts to absorb microwave, to realize common sintering.Synchroballistic Microwave Hybrid co-sintering of the present invention as shown in Fig. 2,
Low temperature low dielectric loss ceramic 3 and the sintering jointly of the high dielectric loss ceramic of low temperature 4, without auxiliary heating body to get
To two kinds and a variety of ceramics.
The present invention absorbs microwave in cold stage using silicon carbide ceramic product, and conducting self-heating simultaneously forms heat source, and radiation is such as
Zirconia ceramic product increases to a certain extent to temperature, and zirconia ceramic product loss improves, and realizes common sintering.
Beneficial effects of the present invention: in the microwave sintering method of single ceramic, it is bound to cause a large amount of energy waste.
It for conventional low-loss ceramic, needs to add auxiliary heating body, this just indirectly increases the consumption of microwave energy；Phase therewith
Answer, room temperature height loss ceramic, during microwave-absorbing heat-generating, its own radiation heat be not also utilized and
It consumes.The present invention provides a kind of synchroballistic Microwave Hybrid cofiring connection, is utilized microwave energy more effectively.Moreover,
Using the two kinds or more of ceramics of microwave once-firing, product structural integrity is burnt into without cracking, hence it is evident that can be improved ceramics
The yield of product.The present invention is applied in the industry of microwave sintering ceramic, will greatly improve production efficiency, improves energy utilization
Rate.
Detailed description of the invention
Fig. 1 is that low-loss ceramic is sintered schematic diagram in the prior art；
Fig. 2 is synchroballistic Microwave Hybrid co-sintering schematic diagram in the present invention；
Fig. 3 is zirconia ceramic product sintering front and back comparison diagram in kind in embodiment 1；
Fig. 4 is silicon carbide ceramic product sintering front and back comparison diagram in kind in embodiment 1；
Fig. 5 is 1 microwave input power of embodiment and temperature profile；
Fig. 6 is zirconia ceramic product microwave sintering front and back comparison diagram in kind in embodiment 2；
Fig. 7 is SEM and XRD diagram after zirconia ceramic product sintering in embodiment 2；
Fig. 8 is zirconia ceramic product microwave sintering front and back comparison diagram in kind in embodiment 3.
Specific embodiment
Only invention is further described in detail for following embodiments, but does not constitute any limitation of the invention.
Embodiment 1
Synchroballistic Microwave Hybrid co-sintering method includes the following steps: in the present embodiment
1) it chooses appropriate matched zirconia ceramic product green body and silicon carbide ceramic product green body is put into heat preservation dress jointly
In setting, it is not necessarily to auxiliary heating body, attemperator is put into the microwave resonance cavity of TE666 mode；Selected zirconia ceramics
Product is zirconia ceramics ring, and consistency is splendid, apparent porosity 0.03%, and selected silicon carbide articles are silicon carbide ceramics
Pipe；
2) microwave input power is adjusted to 2kW, is heated up with the heating rate of 2-18 DEG C/min, when heating rate lower than 2 DEG C/
When min, adjust microwave input power to 4kW, heated up with the heating rate of 2-12 DEG C/min, when heating rate again below 2 DEG C/
When min, input power is adjusted again to 6kW, is warming up to 1550 DEG C；
3) input power is finely tuned, it is made to keep the temperature 30min；
4) power is downgraded into 2kW after keeping the temperature, so that temperature is reduced to 800 DEG C, is then shut off microwave source, Temperature fall.
Sintering temperature, input power are shown in Fig. 5 to the curve graph of time during microwave sintering, as can be seen from Figure 5 micro-
It is gradually slack-off that wave is sintered heating rate, the reason is that organic matter binding agent couples strongly with microwave in cold stage in ceramic body,
Sample is promoted to be rapidly heated before 300 DEG C.With the exclusion of organic matter, heating rate gradually slows down, but does not drop significantly
Low, the reason is that the silicon carbide articles of the high dielectric loss of initial stage of sintering, absorb microwave, self-heating radiations heat energy balances whole liter
Warm rate, after 800 DEG C, with the raising of input power, heating rate keeps balance, illustrate zircite product with microwave coupling
The decrease of the enhancing of conjunction ability and silicon carbide and microwave coupling ability reaches relative equilibrium.
Zirconia ceramics ring sintering front and back comparison is as shown in figure 3, silicon carbide ceramic is burnt in the present embodiment in the present embodiment
The comparison of knot front and back is as shown in figure 4, it is burnt into product structural integrity without cracking.After the completion of sintering, sample does not crack, and illustrates
The wipe-out mode of organic matter and rate are moderate in microwave field, this sintering process can guarantee the intact firing of two kinds of ceramics.
Embodiment 2
Synchroballistic Microwave Hybrid co-sintering method includes the following steps: in the present embodiment
1) it chooses appropriate matched zirconia ceramic product green body and silicon carbide ceramic product green body is put into heat preservation dress jointly
In setting, it is not necessarily to auxiliary heating body, attemperator is put into the microwave resonance cavity of TE666 mode；Selected zirconia ceramics system
Product are zirconia ceramics pipe；
2) microwave input power is adjusted to 1.5kW, is heated up with the heating rate of 2-15 DEG C/min, when heating rate is lower than 2
DEG C/min when, adjust microwave input power to 3.5kW, heated up with the heating rate of 2-10 DEG C/min, when heating rate is low again
When 2 DEG C/min, input power is adjusted again to 5.5kW, is warming up to 1350 DEG C；
3) input power is finely tuned, it is made to keep the temperature 50min；
4) power is downgraded into 1.5kW after keeping the temperature, so that temperature is reduced to 750 DEG C, is then shut off microwave source, Temperature fall.
Zirconia ceramic product sintering front and back comparison is as shown in fig. 6, it is burnt into product structural integrity without cracking in the present embodiment.
SEM and XRD diagram after zirconia ceramic product is sintered in the present embodiment are as shown in fig. 7, it can be seen that oxygen from SEM figure
It is good to change zircon ceramic crystal growth, compact structure, and crystal grain is uniform, it can be seen that tetragonal phase zirconium oxide from XRD diagram (upper right)
Diffractive features peak, peak shape is sharp, in strength set, further illustrates that its crystallization degree is good, corresponding with SEM figure.
Embodiment 3
Synchroballistic Microwave Hybrid co-sintering method includes the following steps: in the present embodiment
1) it chooses appropriate matched zirconia ceramic product green body and silicon carbide ceramic product green body is put into heat preservation dress jointly
In setting, it is not necessarily to auxiliary heating body, attemperator is put into the microwave resonance cavity of TE666 mode；Selected zirconia ceramics system
Product are zirconia ceramics piece；
2) microwave input power is adjusted to 2.5kW, is heated up with the heating rate of 2-20 DEG C/min, when heating rate is lower than 2
DEG C/min when, adjust microwave input power to 4.5kW, heated up with the heating rate of 2-15 DEG C/min, when heating rate is low again
When 2 DEG C/min, input power is adjusted again to 6.5kW, is warming up to 1450 DEG C；
3) input power is finely tuned, it is made to keep the temperature 40min；
4) power is downgraded into 2.5kW after keeping the temperature, so that temperature is reduced to 850 DEG C, is then shut off microwave source, Temperature fall.
Zirconia ceramic product sintering front and back comparison is as shown in figure 8, it is burnt into product structural integrity without cracking in the present embodiment.
Claims (2)
1. a kind of synchroballistic Microwave Hybrid co-sintering method, characterized by the following steps:
1) the high dielectric loss ceramic of low temperature and low temperature low dielectric loss ceramic are put into microwave resonance cavity jointly；
The high dielectric loss ceramic of low temperature is silicon carbide ceramics, and the low temperature low dielectric loss ceramic is zirconium oxide pottery
Porcelain；
2) microwave input power is adjusted to 1.5-2.5kW, when heating rate be lower than 2 DEG C/min when, adjust microwave input power to
3.5-4.5kW adjusts input power to 5.5-6.5kW again, is warming up to 1350- when heating rate is again below 2 DEG C/min
1550℃；
3) input power is finely tuned, it is made to keep the temperature 30-50min；
4) power is then downgraded into 1.5-2.5kW, temperature is made to be reduced to 750-850 DEG C, close microwave source, Temperature fall.
2. synchroballistic Microwave Hybrid co-sintering method according to claim 1, it is characterised in that: by the low temperature Gao Jie
Matter loss ceramic and low temperature low dielectric loss ceramic are put into attemperator jointly, are then put into attemperator micro-
In wave resonance cavity.
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| CN109970447B (en) * | 2019-02-28 | 2021-08-13 | 昆明理工大学 | Ignition method for microwave self-propagating sintering of weak absorption type MAX binding agent |
| CN117945754B (en) * | 2024-01-31 | 2024-09-06 | 江南大学 | Method for preparing ceramic false tooth based on photocuring additive manufacturing and microwave sintering technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1608039A (en) * | 2000-12-29 | 2005-04-20 | 康宁股份有限公司 | Method for processing ceramics using electromagnetic energy |
| CN103467105A (en) * | 2013-08-21 | 2013-12-25 | 田万鸿 | Improvement of zirconia ceramic microwave sintering method and saggar used by same |
| CN104326751A (en) * | 2014-07-01 | 2015-02-04 | 郑州大学 | Microwave sintering method of ZTA ceramic |
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| US5202541A (en) * | 1991-01-28 | 1993-04-13 | Alcan International Limited | Microwave heating of workpieces |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1608039A (en) * | 2000-12-29 | 2005-04-20 | 康宁股份有限公司 | Method for processing ceramics using electromagnetic energy |
| CN103467105A (en) * | 2013-08-21 | 2013-12-25 | 田万鸿 | Improvement of zirconia ceramic microwave sintering method and saggar used by same |
| CN104326751A (en) * | 2014-07-01 | 2015-02-04 | 郑州大学 | Microwave sintering method of ZTA ceramic |
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