CN106673671A - Synchronous compensation microwave hybrid co-sintering method - Google Patents
Synchronous compensation microwave hybrid co-sintering method Download PDFInfo
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- CN106673671A CN106673671A CN201710024851.3A CN201710024851A CN106673671A CN 106673671 A CN106673671 A CN 106673671A CN 201710024851 A CN201710024851 A CN 201710024851A CN 106673671 A CN106673671 A CN 106673671A
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/667—Sintering using wave energy, e.g. microwave sintering
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Abstract
The invention discloses a synchronous compensation microwave hybrid co-sintering method, which belongs to the technical field of microwave sintering ceramic products. The method comprises the following steps: putting a low-temperature ceramic product with a high dielectric loss and a low-temperature ceramic product with a low dielectric loss into a microwave resonant cavity together; carrying out gradient regulation on microwave input power to raise a temperature to 1350-1550DEG C; carrying out fine tuning on the microwave input power, and keeping the temperature for 30-50min; then, lowering the power to 1.5-2.5kw, lowering the temperature to 750-850DEG C, shutting down a microwave source, and naturally cooling. The microwave coupling performance difference of different ceramic products are utilized for realizing the synchronous compensation microwave hybrid co-sintering of the ceramic products, the production efficiency of the ceramic products can be improved, and an energy use ratio can be improved.
Description
Technical field
The present invention relates to a kind of synchroballistic Microwave Hybrid co-sintering method, belongs to microwave sintering ceramic technology neck
Domain.
Background technology
Microwave heating is widely used to daily life as an emerging energy-conservation, efficient, free of contamination sintering technology
In.Ceramic body has to just to make mutually to be bondd between granule through the sintering of high temperature, is formed and has some strength, hardness
Ceramic body.Normal sintering is adopted existing sintering process more, there is sintering period length, low production efficiency, sintering temperature height and energy
The problem that source wastes.Microwave sintering is that the special wave band having using microwave carries out coupling generation heat with material, and material leads to
Cross the dielectric loss of itself absorb electromagnetic energy make it is overall be heated to sintering temperature, with overall heating, uniform heating, selectivity
Heat, be easily controlled, it is energy-efficient the features such as.
At present, the ceramic material of microwave sintering mainly includes, carborundum, 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, its medium
Loss also has very big difference.The difference of dielectric loss causes difference of the ceramic material to microwave absorbing property, so as to cause heating
The difference of effect.By taking zirconia ceramicss as an example, because dielectric loss is relatively low under its room temperature, therefore using the sintering side of auxiliary heating
Formula, makes first auxiliary heating and thermal insulation structure, using the performance of the good absorption microwave of auxiliary heating body room temperature, produces heat,
To zirconia ceramicss radiant heating, to 400 DEG C or so, zirconia media loss is raised, and realizes microwave heating.Same principle,
During sintering to complex phase ceramic, heated using the selectivity of microwave, high lossy medium absorbs microwave in complex phase ceramic, is formed
Internal heat resource, so as to heat low loss dielectric, eventually forms overall heating mode.The method can be avoided using auxiliary heating
Body, but it is only limitted to the sintering of composite ceramic material.
Publication No. discloses a kind of ZTA ceramic microwaves sintering method, the method for CN104326751A Chinese invention patents
Large-sized eccentric ZTA ceramic valves are successfully burnt till using microwave, sintering time has been greatly reduced, while the localized heat for proposing
Amount compensation principle also provides a kind of theoretical foundation for the irregular ceramic of microwave sintering.However, correlation in prior art
Study limitation that is, in a microwave heating cycle, enters in the microwave sintering of single ceramic material only for a kind of ceramic material
Row microwave sintering.The microwave sintering method of this single ceramic, certainly will cause substantial amounts of energy waste.For conventional low damage
Consumption ceramic, needs to add auxiliary heating body, and low-loss ceramic 1 as shown in Figure 1 needs auxiliary heating body 2 to be aided in
Heat-agglomerating, this just indirectly increased the consumption of microwave energy；Correspondingly, the ceramic of the high loss of room temperature, micro- absorbing
During ripple generates heat, the heat of its own radiation is not obtained by yet and consumes.Energy wave during this microwave sintering
The problem taken is badly in need of solving.
The content of the invention
It is an object of the invention 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 realize object above, the technical solution adopted in the present invention is：
A kind of synchroballistic Microwave Hybrid co-sintering method, comprises the steps：
1) the high dielectric loss ceramic of low temperature and low temperature low dielectric loss ceramic are put into into microwave cavity jointly
In body；
2) microwave input power is adjusted to into 1.5-2.5kW, when heating rate is less than 2 DEG C/min, adjusts microwave input work
Rate, when heating rate is again below 2 DEG C/min, adjusts again input power to 5.5-6.5kW to 3.5-4.5kW, is warming up to
1350-1550℃；
3) input power is finely tuned so as to be incubated 30-50min；
4) and then by power 1.5-2.5kW is downgraded, makes temperature be reduced to 750-850 DEG C, close microwave source, dropped naturally
Temperature.
The step 2) in when microwave input power is adjusted to into 1.5-2.5kW, heating rate is 2-20 DEG C/min.
The step 2) in adjust microwave input power to 3.5-4.5kW when, heating rate be 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 into guarantor jointly
In warm device, then attemperator is put in microwave resonance cavity.
The high dielectric loss ceramic of the low temperature is silicon carbide ceramics.
The low temperature low dielectric loss ceramic is zirconia ceramicss.
Preferably, the high dielectric loss ceramic of the low temperature is silicon carbide ceramic.
Preferably, the low temperature low dielectric loss ceramic is zirconia ceramicss pipe, zirconia ceramicss ring, zirconium oxide pottery
Ceramics.
It is further preferred that its consistency of the zirconia ceramicss is splendid, apparent porosity is 0.03%.
During the synchroballistic Microwave Hybrid co-sintering of the present invention, when microwave power is constant, heating rate can gradually become
Slowly, it is therefore desirable to which adjusting microwave input rate, to rise to temperature temperature required.The reason for heating rate is gradually slack-off is ceramic blank
Organic matter binding agent is coupled strongly with microwave in cold stage in body, promotes sample to be rapidly heated before 300 DEG C.With organic
The exclusion of thing, heating rate progressively slows down, but is not greatly lowered, and reason is the carborundum system of the high dielectric loss of initial stage of sintering
Product, absorb microwave, and self-heating radiations heat energy balances overall heating rate, after 800 DEG C, with the raising of input power,
Heating rate keeps balance, illustrates the enhancing with microwave coupling ability and carborundum and the microwave coupling ability of zircite product
Decrease reaches relative equilibrium.
Synchroballistic Microwave Hybrid co-sintering method in the present invention, i.e., using the ceramic of the high dielectric loss of low temperature processed
Good absorbing microwave capability, in cold stage microwave is absorbed, and realizes that conducting self-heating is sintered, and can be as thermal 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 is raised, and starts to absorb microwave, so as 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 is sintered jointly with the high dielectric loss ceramic 4 of low temperature, without the need for auxiliary heating body, is obtained final product
To two kinds and various ceramics.
The present invention absorbs microwave using silicon carbide ceramic product in cold stage, and conducting self-heating simultaneously forms thermal source, and radiation is such as
Zirconia ceramic product, raises to a certain extent to temperature, and zirconia ceramic product loss is improved, and realizes common sintering.
Beneficial effects of the present invention：In the microwave sintering method of single ceramic, substantial amounts of energy waste certainly will be caused.
For conventional low-loss ceramic, need to add auxiliary heating body, this just indirectly increased the consumption of microwave energy；Phase therewith
Should, the ceramic of the high loss of room temperature, during microwave-absorbing heat-generating, heat of its own radiation be not obtained by yet and
Consume.The present invention provides a kind of synchroballistic Microwave Hybrid co-sintering method, microwave energy is more effectively obtained by.And,
Using the two kinds or more of ceramics of microwave once-firing, it burns till product structural integrity without cracking, hence it is evident that can improve 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.
Description of the drawings
Fig. 1 is low-loss ceramic sintering schematic diagram in prior art；
Fig. 2 is synchroballistic Microwave Hybrid co-sintering schematic diagram in the present invention；
Fig. 3 is comparison diagram in kind before and after zirconia ceramic product sintering in embodiment 1；
Fig. 4 is comparison diagram in kind before and after silicon carbide ceramic product sintering in embodiment 1；
Fig. 5 is the microwave input power of embodiment 1 and temperature profile；
Fig. 6 is comparison diagram in kind before and after zirconia ceramic product microwave sintering in embodiment 2；
Fig. 7 is SEM and XRD figure after zirconia ceramic product sintering in embodiment 2；
Fig. 8 is comparison diagram in kind before and after zirconia ceramic product microwave sintering in embodiment 3.
Specific embodiment
Following embodiments are only described in further detail to the present invention, but do not constitute any limitation of the invention.
Embodiment 1
Synchroballistic Microwave Hybrid co-sintering method comprises the steps in the present embodiment：
1) the zirconia ceramic product base substrate and silicon carbide ceramic product base substrate for choosing appropriate matching is put into insulation dress jointly
In putting, without the need for auxiliary heating body, attemperator is put in the microwave resonance cavity of TE666 patterns；Selected zirconia ceramicss
Product is zirconia ceramicss ring, and its consistency is splendid, and apparent porosity is 0.03%, and selected silicon carbide articles are silicon carbide ceramics
Pipe；
2) microwave input power is adjusted to into 2kW, is heated up with the heating rate of 2-18 DEG C/min, when heating rate less than 2 DEG C/
During 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/
During min, input power is adjusted again to 6kW, be warming up to 1550 DEG C；
3) input power is finely tuned so as to be incubated 30min；
4) power is downgraded into 2kW after being incubated, makes temperature be reduced to 800 DEG C, be then shut off microwave source, Temperature fall.
Sintering temperature, input power are shown in Fig. 5 to the curve chart of time during microwave sintering, as can be seen from Figure 5 micro-
Ripple sintering heating rate is gradually slack-off, and reason is that organic matter binding agent is coupled 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 substance, heating rate progressively slows down, but does not significantly drop
Low, reason is the silicon carbide articles of the high dielectric loss of initial stage of sintering, absorbs microwave, and self-heating radiations heat energy balances overall liter
Warm speed, after 800 DEG C, with the raising of input power, heating rate keeps balance, illustrate zircite product with microwave coupling
The enhancing of conjunction ability reaches relative equilibrium with carborundum with the decrease of microwave coupling ability.
Contrast as shown in figure 3, silicon carbide ceramic burns in the present embodiment before and after zirconia ceramicss ring sintering in the present embodiment
Contrast is as shown in figure 4, it burns till product structural integrity without cracking before and after knot.After the completion of sintering, sample is not cracking, illustrates
The wipe-out mode and speed of Organic substance are moderate in microwave field, and this sintering process can ensure that two kinds of the intact of ceramic burn till.
Embodiment 2
Synchroballistic Microwave Hybrid co-sintering method comprises the steps in the present embodiment：
1) the zirconia ceramic product base substrate and silicon carbide ceramic product base substrate for choosing appropriate matching is put into insulation dress jointly
In putting, without the need for auxiliary heating body, attemperator is put in the microwave resonance cavity of TE666 patterns；Selected zirconia ceramicss system
Product are zirconia ceramicss pipe；
2) microwave input power is adjusted to into 1.5kW, is heated up with the heating rate of 2-15 DEG C/min, when heating rate is less 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 it is low again
When 2 DEG C/min, input power is adjusted again to 5.5kW, be warming up to 1350 DEG C；
3) input power is finely tuned so as to be incubated 50min；
4) power is downgraded into 1.5kW after being incubated, makes temperature be reduced to 750 DEG C, be then shut off microwave source, Temperature fall.
Contrast as shown in fig. 6, it burns till product structural integrity without cracking before and after zirconia ceramic product sintering in the present embodiment.
SEM and XRD figure are as shown in fig. 7, it can be seen that oxygen from SEM figures after zirconia ceramic product is sintered in the present embodiment
Change zircon ceramic crystal growth good, compact structure, and crystal grain is uniform, it can be seen that tetragonal phase zirconium oxide from XRD figure (upper right)
Diffractive features peak, peak shape is sharp, in strength set, further illustrates its crystallization degree well, corresponding with SEM figures.
Embodiment 3
Synchroballistic Microwave Hybrid co-sintering method comprises the steps in the present embodiment：
1) the zirconia ceramic product base substrate and silicon carbide ceramic product base substrate for choosing appropriate matching is put into insulation dress jointly
In putting, without the need for auxiliary heating body, attemperator is put in the microwave resonance cavity of TE666 patterns；Selected zirconia ceramicss system
Product are zirconia ceramicss piece；
2) microwave input power is adjusted to into 2.5kW, is heated up with the heating rate of 2-20 DEG C/min, when heating rate is less 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 it is low again
When 2 DEG C/min, input power is adjusted again to 6.5kW, be warming up to 1450 DEG C；
3) input power is finely tuned so as to be incubated 40min；
4) power is downgraded into 2.5kW after being incubated, makes temperature be reduced to 850 DEG C, be then shut off microwave source, Temperature fall.
Contrast as shown in figure 8, it burns till product structural integrity without cracking before and after zirconia ceramic product sintering in the present embodiment.
Claims (4)
1. a kind of synchroballistic Microwave Hybrid co-sintering method, it is characterised in that：Comprise the steps：
1) the high dielectric loss ceramic of low temperature and low temperature low dielectric loss ceramic are put in microwave resonance cavity jointly；
2) microwave input power is adjusted to into 1.5-2.5kW, when heating rate be less than 2 DEG C/min when, adjust microwave input power to
3.5-4.5kW, when heating rate is again below 2 DEG C/min, adjusts again input power to 5.5-6.5kW, is warming up to 1350-
1550℃；
3) input power is finely tuned so as to be incubated 30-50min；
4) and then by power 1.5-2.5kW is downgraded, makes temperature 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 is lost ceramic and is put into jointly in attemperator with low temperature low dielectric loss ceramic, is then put into attemperator micro-
In wave resonance cavity.
3. synchroballistic Microwave Hybrid co-sintering method according to claim 1 and 2, it is characterised in that：The low temperature is high
Dielectric loss ceramic is silicon carbide ceramics.
4. synchroballistic Microwave Hybrid co-sintering method according to claim 1 and 2, it is characterised in that：The low temperature is low
Dielectric loss ceramic is zirconia ceramicss.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216153A (en) * | 2017-06-27 | 2017-09-29 | 广东工业大学 | A kind of 3D printing method of ceramic material |
| CN109970447A (en) * | 2019-02-28 | 2019-07-05 | 昆明理工大学 | A kind of weak ignition method for inhaling the sintering of wave mode MAX bonding agent microwave self- propagating |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5202541A (en) * | 1991-01-28 | 1993-04-13 | Alcan International Limited | Microwave heating of workpieces |
| 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 |
-
2017
- 2017-01-13 CN CN201710024851.3A patent/CN106673671B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5202541A (en) * | 1991-01-28 | 1993-04-13 | Alcan International Limited | Microwave heating of workpieces |
| 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 |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107216153A (en) * | 2017-06-27 | 2017-09-29 | 广东工业大学 | A kind of 3D printing method of ceramic material |
| CN109970447A (en) * | 2019-02-28 | 2019-07-05 | 昆明理工大学 | A kind of weak ignition method for inhaling the sintering of wave mode MAX bonding agent microwave self- propagating |
| 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 |
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| CN106673671B (en) | 2019-08-02 |
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