CN105627760B - A kind of microwave material placing device of high temperature sintering - Google Patents
A kind of microwave material placing device of high temperature sintering Download PDFInfo
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- CN105627760B CN105627760B CN201610075400.8A CN201610075400A CN105627760B CN 105627760 B CN105627760 B CN 105627760B CN 201610075400 A CN201610075400 A CN 201610075400A CN 105627760 B CN105627760 B CN 105627760B
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- microwave
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- powder
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- film trap
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D3/00—Charging; Discharging; Manipulation of charge
- F27D3/0021—Charging; Discharging; Manipulation of charge of ceramic ware
Abstract
The invention discloses a kind of microwave material placing device of high temperature sintering, inside is sequentially provided with internal layer heat-stable ceramic block film trap, outer layer heat-stable ceramic and builds film trap and heat-insulation layer from the inside to the outside provided with microwave acceptor powder bed, microwave acceptor powder bed periphery；Internal layer heat-stable ceramic builds film trap, outer layer heat-stable ceramic and builds film trap and heat-insulation layer upper end open；Internal layer heat-stable ceramic is built receives powder between film trap and outer layer heat-stable ceramic block film trap filled with outer layer microwave；Outer layer insulation cover is provided with heat-insulation layer upper end open；Outer layer insulation cover is provided with infrared measurement of temperature hole, is connected with microwave acceptor powder bed.Microwave material placing device of the present invention is without using overall charge corundum crucible, and device part replacement is convenient, with low cost, and integral heat insulation effect is good, and programming rate is controllable, uniform, and can effectively be heated to 1800 DEG C of temperatures above.
Description
Technical field
The present invention relates to a kind of microwave material placing device for chemical tool part high temperature sintering.
Background technology
Ceramic post sintering is the critical process for determining ceramic final mass.Now widely used resistance-heated furnace, utilizes hair
The radiation and conduction of hot body heat content, allow the ceramic member of inside to be heated to it by the heat radiation of the heating element heater in oven wall
Sintering temperature.But ceramic poor performance, base substrate inside and outside temperature rise it is inconsistent, can be in completely heated up burner hearth ceramic material
Material, it is necessary to make the temperature of whole burner hearth reach design temperature.Meanwhile, in order to produce fissureless product, it is to avoid internal-external temperature difference is big
The influence caused is, it is necessary to which a slow sintering process, often needs the lasting number time of several hours.Research shows, this to add
Hot mode has more than 80% energy loss in surrounding environment, is energy consumption very big heating means.Also, for a long time
Under high-temperature heating, thermal decomposition or diffusion of components change also can often occur for ceramic post sintering part.
Have been developed that with the device and method of microwave sintering ceramics to replace traditional thermal source both at home and abroad, it is various for sintering
High-quality chemical tool, such as silicon nitride, aluminum oxide, aluminium nitride, zirconium oxide, titanium carbide.When microwave is through ceramics, its part
Energy can be absorbed, and be converted into heat, cause workpiece integrally to heat.According to microwave heating principle, mixed uniformly material or advance
Compressing material base, passes through itself absorption to microwave energy（Or dissipate）Certain high temperature is reached, so as to trigger synthesis anti-
Sintering process or should be completed.This causes microwave heating to can be achieved rapidly and uniformly to heat.Reducing the bar of acid extraction
Under part, this can cause while crystal grain thinning tissue, obtain the consistency of higher workpiece.
Although however, this technology has shown the incomparable advantage of conventional sintering technique, having predictive of it wide
General development prospect.But Microwave Sintering Techniques are in industrial applications still also in initial stage.Microwave Sintering Techniques insulation dress
Install to haggle over and commonly whole carborundum, or the suction microwave powder of activated carbon be placed in attemperator in the inner chamber of one,
Silicon carbide rod is either fixed on crucible surrounding.The high sintering temperature that sintering needs during preparing chemical tool material,
Such as sinter Al2O3Tool piece with TiC, SiN often need to be at 1600-2000 DEG C.Such sintering is required to special microwave charge
The design of heating chamber device proposes more stringent requirement, particularly when microwave charge heating carrier amount is higher.Microwave current
Charge heater still suffers from application problem.Main the problem of, includes:
1）It is difficult to reach up to 1800 DEG C of sintering temperature, programming rate is slow, and firing rate is difficult to control；And high temperature rank
Section non-uniform temperature, continues heat temperature raising difficulty, and micro-wave oven needs extra higher power increase.
2) in microwave heating and cooling procedure, particularly when microwave high-temperature sinters chemical tool, microwave absorption is contained
The corundum crucible of material, often ftractures.
3）After high temperature sintering, the soldering of microwave absorption powder influences powder and the pottery of sintering after-contraction into agglomerate in powder bed
Close contact between porcelain piece surface, causes the uneven of workpiece and insufficient heating.
4）In the high temperature sintering stage, such as larger than 1500 DEG C, the part of ceramic member constitutes phase decomposition or oxidation, and sintered part is most
Whole density reduction.
The content of the invention
The invention aims to solve defect present in prior art can be effectively incubated there is provided one kind, heating
Uniformly, heat up controllable microwave material placing device.
In order to achieve the above object, the invention provides a kind of microwave material placing device of high temperature sintering, the microwave charge
Provided with microwave acceptor powder bed inside device, workpiece is placed in microwave acceptor powder bed and is sintered；Wherein, microwave acceptor powder bed periphery
Internal layer heat-stable ceramic is sequentially provided with from the inside to the outside builds film trap, outer layer heat-stable ceramic block film trap and heat-insulation layer；Internal layer heat-stable ceramic is built
Film trap, outer layer heat-stable ceramic build film trap and heat-insulation layer upper end open；Internal layer heat-stable ceramic builds film trap and outer layer heat-stable ceramic builds piece
Receive powder filled with outer layer microwave between groove；Outer layer insulation cover is provided with heat-insulation layer upper end open；Outer layer insulation cover is provided with
Infrared measurement of temperature hole, is connected with microwave acceptor powder bed.
Inner core microwave receives powder and uses aluminum oxide, graphite and activated carbon with volume ratio 70:15:The mixed powder of 15 compositions
End；Outer layer microwave receives powder and uses carborundum, graphite and activated carbon with volume ratio 60:20:The mixed-powder of 20 compositions.
Outer layer microwave receives powder and may also include micro high lossy microwave material powder；High microwave consume material is selected from
Fe3O4、SnO2、MnO2Or Cr2O3；The high lossy microwave material powder accounts for outer layer microwave receives powder gross weight 1%.
Inner core microwave receives powder and outer layer microwave receives the particle size of powder for micron order.
Above-mentioned heat-insulation layer includes alumina fibre cotton layer, Alumina Foam brick layer and mullite casing successively from the inside to the outside；
Outer layer insulation cover uses mullite lid.
Internal layer heat-stable ceramic build film trap, outer layer heat-stable ceramic build film trap, alumina fibre cotton layer, Alumina Foam brick layer and
Mullite casing is square, and upper end open.
Alumina fibre cotton lid is provided with Alumina Foam brick layer upper end open；Alumina fibre cotton lid is located at mullite lid
Lower section；Alumina fibre cotton is covered provided with infrared measurement of temperature hole, and the infrared measurement of temperature hole that mullite is covered passes through alumina fibre cotton lid
On infrared measurement of temperature hole be connected with microwave acceptor powder bed.
The pore size in above-mentioned infrared measurement of temperature hole is 10mm.
Internal layer heat-stable ceramic builds film trap and outer layer heat-stable ceramic builds film trap and uses aluminum oxide, boron nitride or nitridation silicon chip to interlock
Pile up and form.
The present invention has advantages below compared with prior art：
1st, alumina fibre cotton layer, Alumina Foam brick layer, the mullite casing that the present invention is selected have good wave transparent
Property, resistance to elevated temperatures and low heat conductivity, and by this triple seal, the presence in gap is reduced to the full extent, therefore
Device integral heat insulation effect is good, sintering velocity is fast.Combine, quickly can arrive heating ceramic part with selected multistage coupling loss heating
More than 1800 DEG C；Can uniform heating ceramic part in the larger context in microwave heating powder.
2nd, traditional material placing device carries ceramic member in sintering process and the corundum crucible of heating powder easily ftractures,
Particularly when high temperature sintering is ceramic.By the present invention in that the groove carrying loss heating tiled that interlocked with heat-stable ceramic block piece
Microwave receives filler（Receive powder including inner core microwave and outer layer microwave receives powder）, it is to avoid other microwave bogeys are normal
The corundum crucible problems of crack seen.
3rd, body inner core microwave of the present invention receives powder and outer layer microwave receives difference of the powder to the absorbent properties of microwave,
Can be to low temperature and high temperature different phase sintered body（Workpiece）Heating rate carries out significantly more efficient control：In cold stage, mainly
There is outer layer microwave to receive powder（Carborundum, graphite and activated carbon）Heat energy is generated with microwave coupling, and aids in inner core microwave to receive
The temperature rise of powder；After temperature rises to 800 DEG C, the main body aluminum oxide that inner core microwave receives in powder starts and microwave coupling
Close loss heat.This specific admixture mode of heating, can make workpiece have relatively gentle speed heating, prevent because of gas in cold stage
Body discharge acutely causes workpiece to ftracture；In hot stage, because inner core microwave receives powder and ceramic body（Workpiece）In
Al2O3Start to couple with microwave, the temperature of internal layer can continue stable rise.Inner core microwave of the present invention receives to contain in powder
A small amount of heat-resisting dispersed phase（Graphite and activated carbon）Presence, and granularity is in micron order mixed powder, can hinder main body microwave coupling
Condensation material（Al2O3）Soldering, aggregation and sintering in high temperature, this can ensure the mobility of powder, and ensure close with workpiece surface
Cut-grafting is touched, so that heating is more uniform, effective.Simultaneously because the presence of micron order mixed powder so that inner core microwave receives
There is microvoid and breathable inside powder, it is easy to the introducing of protective atmosphere, in high-temperature sintering process can hinder sintered part
Thermal decomposition or oxidation that composition in ceramic member mutually occurs.
4th, microwave material placing device of the present invention is without using overall charge corundum crucible, device part replacement is convenient, into
This is cheap, and integral heat insulation effect is good, and programming rate is controllable, uniform, and can effectively be heated to 1800 DEG C of temperatures above.Utilize this hair
The ceramic member sintered density that bright material placing device is obtained after being sintered to chemical tool part is above 95%, or even up to
98%。
Brief description of the drawings
Fig. 1 is the structural representation of the microwave material placing device of high temperature sintering of the present invention.
In figure, 1- mullite casings, 2- Alumina Foam brick layer, 3- alumina fibres cotton layer, 4- outer layers heat-stable ceramic is built
Film trap, 5- outer layer microwaves receive powder, and 6- internal layers heat-stable ceramic builds film trap, 7- infrared measurement of temperature hole, 8- mullite lids, 9- aluminum oxide
Cellucotton lid, 10- ceramic post sintering parts, 11- inner core microwaves receive powder.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
Device embodiment
As shown in figure 1, microwave material placing device of the present invention includes mullite casing 1, Alumina Foam brick layer 2, aluminum oxide fibre
Vinylon and cotton blend layer 3, outer layer heat-stable ceramic build film trap 4, internal layer heat-stable ceramic and build film trap 6, mullite lid 8, alumina fibre cotton lid 9.Its
Middle mullite casing 1 and mullite lid 8 constitute the outermost layer of device, and mullite lid 8 is located at the upper of mullite casing 1
Side.In the mullite casing 1 from it is outer and it is interior be sequentially provided with Alumina Foam brick layer 2, alumina fibre cotton layer 3, collectively form this
The heat-insulation layer of device.Oxidized fibre cotton lid 9 is provided with the lower section of the top of Alumina Foam brick layer 2, mullite lid 8, with not coming
Stone lid 8 is collectively forming the lid of the present apparatus.Outer layer heat-stable ceramic is sequentially provided with from outside to inside inside alumina fibre cotton layer 3 builds piece
Groove 4, internal layer heat-stable ceramic build film trap 6, and internal layer heat-stable ceramic is built in film trap 6 receives powder 11 provided with inner core microwave, and outer layer is heat-resisting
Ceramics are built receives powder 5 between film trap 6 and outer layer heat-stable ceramic block film trap 4 provided with outer layer microwave.The He of alumina fibre cotton lid 9
The center of mullite lid 8 is equipped with infrared measurement of temperature hole 7（Diameter is about 10mm）, the center line in two infrared measurement of temperature holes 7 is mutually overlapping
Close, and be connected with the inside that internal layer heat-stable ceramic builds film trap 6.Ceramic post sintering part 10 is placed on internal layer heat-stable ceramic and builds film trap 6
It is interior, bury and overlay on inner core microwave and receive in powder 11.
Wherein, the outer layer microwave that outer layer heat-stable ceramic is built in film trap 4 receives powder 5 for carborundum, graphite and activated carbon
The micron order mixed-powder of composition, its volume ratio is 60:20:20.Micro high lossy microwave material powder can be added in right amount（Plus
Enter amount and receive 1% or so of powder gross weight for outer layer microwave）To improve firing rate, high microwave consume material is selected from Fe3O4、
SnO2、MnO2Or Cr2O3。
It is aluminum oxide, graphite and activated carbon composition that the inner core microwave that internal layer heat-stable ceramic is built in film trap 6, which receives powder 11,
Micron order mixed-powder, its volume ratio be 70:15:15.
Outer layer heat-stable ceramic builds film trap 4 and internal layer heat-stable ceramic builds film trap 6 and uses resistant to elevated temperatures corundum piece or silicon nitride
Piece, is staggeredly tiled and forms, and the volume tiled is determined according to the size and number of sintered ceramic member 10.
Application Example 1
The sintering of alumina-based ceramic material.
Raw material is from self-control sintering Al2O3Base ceramic body, main chemical compositions are micron-sized 30 wt% TiC, sub-micro
The molybdenum powder 2wt% of meter level, nickel powder is 4 wt% and TiB 1wt%, sintering aid Y2O, MgO are 1.5 wt%, and main body surplus is Asia
Micron-sized α-Al2O3.It is 13*13*7mm to sinter ceramic single-piece size.By sample to be sintered（Sinter ceramic member 10）Place
Built in internal layer heat-stable ceramic in film trap 6, powder 11 is received with inner core microwave inside groove and is filled up completely with, then internal layer heat-stable ceramic is built
Film trap 6 is put into receives powder 5 with outer layer microwave.The outer layer heat-stable ceramic of filling builds film trap 4（The outer layer heat-stable ceramic builds film trap 4
Portion is sequentially provided with alumina fibre cotton layer 3, Alumina Foam brick layer 2 and mullite casing 1）It is interior.And it is fine to cover aluminum oxide successively
Vinylon and cotton blend lid 9 and mullite lid 8.Microwave material placing device of the present invention is put into the microwave resonance intracavitary of vacuum microwave sintering furnace, adjusted
The relative position of good infrared radiation thermometer and ceramic body（Ensure that infrared light passes through the infrared measurement of temperature inspecting hole 7 of lid, then directly penetrate
To the top on ceramic body surface）, microwave power supply is opened, input power, the heating master of microwave in cold stage, cavity is adjusted
To receive powder 5 dependent on outer layer microwave.And internal layer heat-stable ceramic is built in film trap 6, inner core microwave receives the main body in powder 11
Aluminum oxide, then after its receptor temperature reaches 800 DEG C, start to receive microwave generation loss heating.This specific admixture mode of heating, makes
Heeling-in receives the ceramic body in powder in inner core microwave, cold stage can relatively gentle speed heating, prevent because of gas
Body discharge acutely causes sample to ftracture；And in hot stage, because inner core microwave receives Al in powder 11 and ceramic body2O3Open
Beginning is coupled with microwave, and the temperature of internal layer can be raised continually and steadily.This can ensure the stabilization of the product quality of final ceramics.
Open after microwave, just reached 1600 DEG C in the temperature of 50min or so time sintered specimen, be then incubated 10min, entirely
Sintering process lasts after the completion of about 60min or so, sintering, furnace cooling to room temperature.Its consistency reaches more than 99.2%, surface
Hardness is 21GPa, and bending strength is 918MPa, and fracture toughness is 5.26 MPa m1/2, sintex can have been met to performance
Use requirement.
Application Example 2
Al2O3The dispensing of base ceramic body, charging arrangement and microwave receive powder with Application Example 1.Open after microwave,
In 50min or so the different heats of time control two temperature of sintered specimen heat respectively reached 1500 DEG C, 1700
DEG C, then it is incubated 10min.After the completion of sintering, furnace cooling to room temperature.Different heats have sintered ceramic body, with most high fever
Junction temperature increases, and its consistency is respectively 97.3% and 99.6%, case hardness is respectively 18.6GPa and 22.3G
A, bending strength is respectively 880MPa and 950MPa, and fracture toughness is 3.75 MPa m1/2 With 5.76MPa m1/2。
Use requirement of the sintex to performance can have been met.
Application Example 3
Al2O3The dispensing of base ceramic body, charging arrangement and microwave receive powder with Application Example 1.Add in right amount micro
Cr2O3Powder receives in powder in inner core microwave.Open microwave after, 50min or so time sintered specimen temperature just
1800 DEG C have been reached, 10min is then incubated, whole sintering process lasts after the completion of about 60min or so, sintering, and furnace cooling is arrived
Room temperature.The relative density of obtained sintered specimen is 99.2%, and hardness is 21.6 GPa, and bending strength is 900MPa, fracture
Toughness is 4.26 MPa m1/2, use requirement of the sintex to performance can have been met.
Microwave vacuum sintering furnace microwave frequency is 2.45GHz in the various embodiments described above, in sintering, is passed through hydrogeneous 6% nitrogen
Atmosphere.Peak power output is 5KW.6 magnetrons are respectively above and below microwave cavity, it is ensured that microwave field distribution is equal
It is even.Infrared radiation thermometer can monitor sample temperature in resonator in real time, and measured temperature scope is 350 DEG C ~ 1800 DEG C.
From the foregoing, it will be observed that the device of the present invention can be born compared with high sintering temperature, and uniformity of temperature profile, in addition with liter
Warm velocity-stabilization, good heat insulating is simple in construction, and heating process is easily-controllable, the characteristics of with low cost, can be effectively improved production
Efficiency, while the product comprehensive mechanical property of sintering is higher, meets the use requirement of cutter material.Fully meet microwave sintering use
The requirement of attemperator, with very high practical value.
Claims (8)
1. provided with microwave acceptor powder bed, workpiece inside a kind of microwave material placing device of high temperature sintering, the microwave material placing device
It is placed in the microwave acceptor powder bed and is sintered；It is characterized in that：The microwave acceptor powder bed periphery is set successively from the inside to the outside
There is internal layer heat-stable ceramic to build film trap, outer layer heat-stable ceramic and build film trap and heat-insulation layer；It is resistance to that the internal layer heat-stable ceramic builds film trap, outer layer
Thermal Ceramics build film trap and heat-insulation layer upper end open；The internal layer heat-stable ceramic is built and filled out between film trap and outer layer heat-stable ceramic block film trap
Receive powder filled with outer layer microwave；Outer layer insulation cover is provided with the heat-insulation layer upper end open；The outer layer insulation cover is provided with
Infrared measurement of temperature hole, is connected with microwave acceptor powder bed；The microwave acceptor powder bed receives powder using inner core microwave；The inner core
Microwave receives powder and uses aluminum oxide, graphite and activated carbon with volume ratio 70:15:The mixed-powder of 15 compositions；The outer microtube
Ripple receives powder and uses carborundum, graphite and activated carbon with volume ratio 60:20:The mixed-powder of 20 compositions.
2. microwave material placing device according to claim 1, it is characterised in that：The outer layer microwave receives powder also including micro-
The high lossy microwave material powder of amount；The high microwave consume material is selected from Fe3O4、SnO2、MnO2Or Cr2O3；The high microwave
Loss material powder accounts for outer layer microwave receives powder gross weight 1%.
3. microwave material placing device according to claim 1, it is characterised in that：The inner core microwave receives powder and outer microtube
The particle size that ripple receives powder is micron order.
4. microwave material placing device according to claim 1 or 2, it is characterised in that：The heat-insulation layer is wrapped successively from the inside to the outside
Include alumina fibre cotton layer, Alumina Foam brick layer and mullite casing；The outer layer insulation cover uses mullite lid.
5. microwave material placing device according to claim 4, it is characterised in that：The internal layer heat-stable ceramic builds film trap, outer layer
Heat-stable ceramic is built film trap, alumina fibre cotton layer, Alumina Foam brick layer and mullite casing and is square, and upper end open.
6. microwave material placing device according to claim 5, it is characterised in that：At the Alumina Foam brick layer upper end open
Provided with alumina fibre cotton lid；The alumina fibre cotton lid is located at below the mullite lid；The alumina fibre cotton lid
Be provided with infrared measurement of temperature hole, the infrared measurement of temperature hole that the infrared measurement of temperature hole that the mullite is covered is covered by alumina fibre cotton with
The microwave acceptor powder bed is connected.
7. microwave material placing device according to claim 6, it is characterised in that：The pore size in the infrared measurement of temperature hole is
10mm。
8. microwave material placing device according to claim 1 or 2, it is characterised in that：The internal layer heat-stable ceramic build film trap and
Outer layer heat-stable ceramic block film trap interlocks to pile up using aluminum oxide, boron nitride or nitridation silicon chip to be formed.
Priority Applications (1)
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| CN201610075400.8A CN105627760B (en) | 2016-02-03 | 2016-02-03 | A kind of microwave material placing device of high temperature sintering |
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| CN201610075400.8A CN105627760B (en) | 2016-02-03 | 2016-02-03 | A kind of microwave material placing device of high temperature sintering |
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| CN107664308A (en) * | 2016-07-28 | 2018-02-06 | 南京理工大学 | A kind of simple vacuum microwave oven apparatus |
| CN108731475B (en) * | 2017-04-20 | 2019-10-18 | 南京理工大学 | A kind of ceramic material microwave sintering attemperator |
| CN107716927B (en) * | 2017-10-12 | 2019-10-25 | 钢铁研究总院 | A kind of identical temperature field multichannel honeycomb array crucible |
| CN110822899B (en) * | 2019-11-07 | 2021-03-02 | 南京理工大学 | Auxiliary heating and heat insulating device for microwave sintering |
| CN113418393A (en) * | 2021-07-12 | 2021-09-21 | 郑州大学 | Energy-saving heat-insulating device for microwave kiln and preparation method |
| CN115838291A (en) * | 2022-10-26 | 2023-03-24 | 山东大学 | Method for rapidly synthesizing high-entropy carbonitride ceramic powder by adopting microwaves |
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| JP3145250B2 (en) * | 1994-06-03 | 2001-03-12 | 新日本製鐵株式会社 | How to refill powder into the powder injection tank |
| CN101017058A (en) * | 2007-02-14 | 2007-08-15 | 哈尔滨工业大学 | Microwave sintering material placing device |
| CN104944929B (en) * | 2015-06-05 | 2017-03-22 | 郑州大学 | Microwave sintering method for alumina ceramic balls and auxiliary heating device |
| CN105091604A (en) * | 2015-08-24 | 2015-11-25 | 南京理工大学 | Thermal insulation and auxiliary heating device for microwave sintering of ceramic cutter material |
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