CN105627760A - Microwave storing device for high-temperature sintering - Google Patents
Microwave storing device for high-temperature sintering Download PDFInfo
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- CN105627760A CN105627760A CN201610075400.8A CN201610075400A CN105627760A CN 105627760 A CN105627760 A CN 105627760A CN 201610075400 A CN201610075400 A CN 201610075400A CN 105627760 A CN105627760 A CN 105627760A
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- microwave
- heat
- layer
- outer layer
- film trap
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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 microwave storing device for high-temperature sintering. A microwave powder receiving bed is arranged in the microwave storing device. An inner-layer heat-resistant ceramic brick piece tank, an outer-layer heat-resistant ceramic brick piece tank and a heat preservation layer are arranged on the periphery of the microwave powder receiving bed in sequence from inside to outside. The upper end of the inner-layer heat-resistant ceramic brick piece tank, the upper end of the outer-layer heat-resistant ceramic brick piece tank and the upper end of the heat preservation layer are open. The space between the inner-layer heat-resistant ceramic brick piece tank and the outer-layer heat-resistant ceramic brick piece tank is filled with an outer-layer microwave powder receiving body. An outer-layer heat preservation cover is arranged at the opening in the upper end of the heat preservation layer. The outer-layer heat preservation cover is provided with an infrared temperature measurement hole and communicates with the microwave powder receiving bed. According to the microwave storing device, an integrated storing corundum crucible is not needed; components of the device can be replaced conveniently, and the cost is low; the overall heat preservation effect is good, the temperature increasing rate is controllable and uniform, and the device can be effectively heated to the temperature of 1800 DEG C or over.
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 determining pottery final mass. Now widely used resistance-heated furnace, utilizes radiation and the conduction of heater heat, allows the ceramic member of inside be heated to its sintering temperature by the heat radiation of the heating element heater in oven wall. But ceramic poor performance, it is inconsistent that base substrate inside and outside temperature rises, and the ceramic material in the completely heated up burner hearth of energy, 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 the impact that internal-external temperature difference causes greatly, it is necessary to a sintering process slowly, often need to continue to count the time of several hours. Research shows, this mode of heating has in the energy loss environment around of more than 80%, is the heating means that energy consumption is very big. Further, under long-time high-temperature heating, also often can there is thermal decomposition or diffusion of components change in ceramic post sintering part.
Have been developed that both at home and abroad and replace traditional thermal source with the Apparatus and method for of microwave sintering pottery, be used for sintering various high-quality chemical tool, such as silicon nitride, aluminium oxide, aluminium nitride, zirconium oxide, titanium carbide etc. When microwave is through pottery, its portion of energy can be absorbed, and is converted into heat, causes workpiece entirety to heat. According to microwave heating principle, mixed uniformly material or material base compressing in advance, by self, the absorption (or dissipation) of microwave energy is reached certain high temperature, thus causing synthetic reaction or completing sintering process. This makes microwave heating can realize heating rapidly and uniformly. When reducing acid extraction, this may result in while crystal grain thinning tissue, it is thus achieved that the consistency of higher workpiece.
But, although this technology has shown the advantage that conventional sintering technique is incomparable, predictive of it, there is development prospect widely. But Microwave Sintering Techniques in industrial applications still also in initial stage. The design of Microwave Sintering Techniques attemperator is more typically by whole carborundums, or the microwave powder body of inhaling of activated carbon is placed in attemperator in the inner chamber of, or silicon carbide rod is fixed on crucible surrounding. Sintering prepares the high sintering temperature needed in the process of chemical tool material, such as sintering Al2O3Often need at 1600-2000 DEG C with the tool piece of TiC, SiN. Such sintering requires the design of special microwave charge heating chamber device is proposed more stringent requirement, particularly when microwave charge heating carrier amount is higher. Microwave current charge heater still suffers from application problem. Main problem includes:
1) being difficult to reach the sintering temperature of up to 1800 DEG C, programming rate is slow, and firing rate is wayward; And hot stage non-uniform temperature, continuing heat temperature raising difficulty, microwave oven needs extra higher power to increase.
2) in microwave heating and cooling procedure, particularly when microwave high-temperature sintered ceramic instrument, contain the corundum crucible of microwave absorption material, often ftracture.
3) after high temperature sintering, in powder bed, the seam of microwave absorption powder body becomes agglomerate, affects the close contact between the ceramic member surface of powder body and sintering after-contraction, causes the uneven and insufficient heating of workpiece.
4) in the high temperature sintering stage, as more than 1500 DEG C, the part of ceramic member forms phase decomposition or oxidation, the final densities of sintered part reduces.
Summary of the invention
The invention aims to the defect solving exist in prior art, it is provided that one can effectively be incubated, homogeneous heating, the microwave material placing device heating up controlled.
In order to achieve the above object, the invention provides the microwave material placing device of a kind of high temperature sintering, be provided with microwave receptor powder bed inside this microwave material placing device, workpiece is placed in microwave receptor powder bed and is sintered; Wherein, microwave receptor powder bed periphery is sequentially provided with internal layer heat-stable ceramic from the inside to the outside and builds film trap, outer layer heat-stable ceramic block film trap and heat-insulation layer; Internal layer heat-stable ceramic builds film trap, outer layer heat-stable ceramic builds film trap and heat-insulation layer upper end open; It is filled with outer layer microwave between internal layer heat-stable ceramic block film trap and outer layer heat-stable ceramic block film trap and accepts powder body; Heat-insulation layer upper end open place is provided with outer layer insulation cover; Outer layer insulation cover is provided with infrared measurement of temperature hole, is connected with microwave receptor powder bed.
Inner core microwave accepts powder body and adopts aluminium oxide, graphite and activated carbon with the volume ratio 70:15:15 mixed-powder formed; Outer layer microwave accepts powder body and adopts carborundum, graphite and activated carbon with the volume ratio 60:20:20 mixed-powder formed.
Outer layer microwave accepts powder body and may also include the high lossy microwave material powder of trace; High microwave consume material is selected from Fe3O4��SnO2��MnO2Or Cr2O3; Described high lossy microwave material powder accounts for outer layer microwave and accepts the 1% of powder body gross weight.
Inner core microwave accepts powder body and outer layer microwave to accept the size of powder body be micron order.
Above-mentioned heat-insulation layer includes alumina fibre cotton layer, Alumina Foam brick layer and mullite casing from the inside to the outside successively; Outer layer insulation cover adopts mullite lid.
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 all square, and upper end open.
Alumina Foam brick layer upper end open place is provided with alumina fibre cotton lid; Alumina fibre cotton lid is positioned at below mullite lid; Alumina fibre cotton covers and is provided with infrared measurement of temperature hole, and the infrared measurement of temperature hole that the infrared measurement of temperature hole on mullite lid is covered by alumina fibre cotton is connected with microwave receptor powder bed.
The pore size in above-mentioned infrared measurement of temperature hole is 10mm.
Internal layer heat-stable ceramic is built film trap and outer layer heat-stable ceramic and is built film trap and adopt aluminium oxide, boron nitride or nitrogenize staggered the piling up of silicon chip and form.
The present invention has the advantage that compared to existing technology
1, the present invention selects alumina fibre cotton layer, Alumina Foam brick layer, mullite casing have good wave, resistance to elevated temperatures and low heat conductivity, and by this triple seal, decreasing the existence in gap to the full extent, therefore device integral heat insulation is effective, sintering velocity is fast. Combine with the heating of selected multistage coupling loss, can quick heating ceramic part to more than 1800 DEG C; Can uniform heating ceramic part in the larger context in microwave heating powder body.
2, tradition material placing device carry in sintering process ceramic member and heating powder body corundum crucible be susceptible to ftracture, particularly when high temperature sintering pottery. By the present invention in that building the sheet groove carrying loss heating microwave tiled that interlocks with heat-stable ceramic accepts filler (include inner core microwave accept powder body and outer layer microwave accepts powder body), it is to avoid the corundum crucible problems of crack that other microwave bogeys are common.
3, body inner core microwave of the present invention accepts powder body and outer layer microwave accepts the powder body difference to the absorbent properties of microwave, low temperature and high temperature different phase sintered body (workpiece) heating rate can be carried out significantly more efficient control: at cold stage, mainly there is outer layer microwave to accept powder body (carborundum, graphite and activated carbon) and generate heat energy with microwave coupling, and assist the temperature that inner core microwave accepts powder body to raise; After temperature rises to 800 DEG C, inner core microwave accepts the main body aluminium oxide in powder body and starts heat raw with microwave coupling loss. This specific admixture mode of heating, can make workpiece have relatively mild speed to heat up at cold stage, it is prevented that discharges because of gas and acutely causes that workpiece ftractures; At hot stage, accept the Al in powder body and ceramic body (workpiece) due to inner core microwave2O3Starting to couple with microwave, the temperature of internal layer can continue stable rising. Inner core microwave of the present invention accepts the existence in powder body containing a small amount of heat-resisting dispersion phase (graphite and activated carbon), and granularity is at micron order mixed powder, can hinder main body microwave coupling material (Al2O3) seam when high temperature, gathering and sintering, this can ensure the mobility of powder body, and ensures and surface of the work close contact so that heating more uniformly, effective. Simultaneously because the existence of micron order mixed powder so that inner core microwave accepts there is microvoid and breathable inside powder body, it is easy to the introducing of protective atmosphere, thermal decomposition that the composition that can hinder in sintered part in ceramic member at high-temperature sintering process occurs mutually or oxidation.
4, microwave material placing device of the present invention is without using the charge corundum crucible of entirety, and device part replacement is convenient, with low cost, and integral heat insulation is effective, and programming rate is controlled, uniform, and can effectively heat to 1800 DEG C of temperatures above. Utilize the ceramic member sintered density that material placing device of the present invention obtains after chemical tool part is sintered to be above 95%, even may be up to 98%.
Accompanying drawing explanation
Fig. 1 is the structural representation of the microwave material placing device of high temperature sintering of the present invention.
In figure, 1-mullite casing, 2-Alumina Foam brick layer, 3-alumina fibre cotton layer, 4-outer layer heat-stable ceramic builds film trap, 5-outer layer microwave accepts powder body, and 6-internal layer heat-stable ceramic builds film trap, 7-infrared measurement of temperature hole, 8-mullite lid, 9-alumina fibre cotton lid, 10-ceramic post sintering part, 11-inner core microwave accepts powder body.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in detail.
Device embodiment
As it is shown in figure 1, microwave material placing device of the present invention includes mullite casing 1, Alumina Foam brick layer 2, alumina fibre cotton layer 3, outer layer heat-stable ceramic builds film trap 4, internal layer heat-stable ceramic builds film trap 6, mullite lid 8, alumina fibre cotton lid 9. Wherein mullite casing 1 and mullite lid 8 constitute the outermost layer of device, and mullite lid 8 is positioned at the top of mullite casing 1. In mullite casing 1 from outer and in be sequentially provided with Alumina Foam brick layer 2, alumina fibre cotton layer 3, collectively form the heat-insulation layer of this device. Above Alumina Foam brick layer 2, mullite lid 8 be connected with oxidized fibre cotton lid 9, with the lid that mullite lid 8 is collectively forming this device. The internal outer layer heat-stable ceramic that is sequentially provided with from outside to inside of alumina fibre cotton layer 3 builds film trap 4, internal layer heat-stable ceramic block film trap 6, it is provided with inner core microwave in internal layer heat-stable ceramic block film trap 6 and accepts powder body 11, be provided with outer layer microwave between outer layer heat-stable ceramic block film trap 6 and outer layer heat-stable ceramic block film trap 4 and accept powder body 5. The center of alumina fibre cotton lid 9 and mullite lid 8 is equipped with infrared measurement of temperature hole 7(diameter and is about 10mm), the centrage in two infrared measurement of temperature holes 7 coincides, and the inside building film trap 6 with internal layer heat-stable ceramic is connected. Ceramic post sintering part 10 is placed on internal layer heat-stable ceramic and builds in film trap 6, buries and overlays on inner core microwave and accept in powder body 11.
Wherein, outer layer heat-stable ceramic is built the outer layer microwave in film trap 4 and is accepted the micron order mixed-powder that powder body 5 is carborundum, graphite and activated carbon composition, and its volume ratio is 60:20:20. Can adding the high lossy microwave material powder (addition is that outer layer microwave accepts about the 1% of powder body gross weight) of trace in right amount to improve firing rate, high microwave consume material is selected from Fe3O4��SnO2��MnO2Or Cr2O3��
Internal layer heat-stable ceramic is built the inner core microwave in film trap 6 and is accepted the micron order mixed-powder that powder body 11 is aluminium oxide, graphite and activated carbon composition, and its volume ratio is 70:15:15.
Outer layer heat-stable ceramic builds film trap 4 and internal layer heat-stable ceramic is built film trap 6 and adopted resistant to elevated temperatures corundum sheet or nitrogenize silicon chip, and staggered tiling forms, and the volume tiled is determined according to size and the quantity of institute's sintered ceramic part 10.
Application Example 1
The sintering of alumina-based ceramic material.
Self-control sintering Al selected by raw material2O3Base ceramic body, main chemical compositions is micron-sized 30wt%TiC, and the molybdenum powder 2wt% of submicron order, nikel powder is 4wt% and TiB1wt%, sintering aid Y2O, MgO are 1.5wt%, and main body surplus is the ��-Al of submicron order2O3. Institute's sintered ceramic single-piece is of a size of 13*13*7mm. Sample to be sintered (i.e. sintered ceramic part 10) being positioned over internal layer heat-stable ceramic build in film trap 6, accept powder body 11 with inner core microwave and be filled up completely with inside groove, then internal layer heat-stable ceramic block film trap 6 is put into and is accepted powder body 5 with outer layer microwave. The outer layer heat-stable ceramic filled is built this outer layer heat-stable ceramic of film trap 4(block film trap 4 and is sequentially provided with alumina fibre cotton layer 3, Alumina Foam brick layer 2 and mullite casing 1) in. And build alumina fibre cotton lid 9 and mullite lid 8 successively. Microwave material placing device of the present invention is put into the microwave resonance intracavity of vacuum microwave sintering furnace, adjust relative position (the infrared measurement of temperature inspecting hole 7 of guarantee infrared light traverse lid of infrared radiation thermometer and ceramic body, then the top on ceramic body surface directly it is mapped to), open microwave power supply, regulate input power, in cold stage, cavity, the heating of microwave depends on outer layer microwave and accepts powder body 5. And internal layer heat-stable ceramic is built in film trap 6, inner core microwave accepts the main body aluminium oxide in powder body 11, then, after its receptor temperature reaches 800 DEG C, start to accept microwave generation loss heating. This specific admixture mode of heating, makes heeling-in accept the ceramic body in powder body at inner core microwave, and speed that can be relatively mild at cold stage heats up, it is prevented that discharges because of gas and acutely causes that sample ftractures; And at hot stage, accept Al in powder body 11 and ceramic body due to inner core microwave2O3Starting to couple with microwave, the temperature of internal layer can raise continually and steadily. This can ensure stablizing of final ceramic product quality. Opening after microwave, the temperature at the time sintered specimen of about 50min has just reached 1600 DEG C, is incubated 10min subsequently, and whole sintering process continues about about 60min, and after having sintered, furnace cooling is to room temperature. Its consistency reaches more than 99.2%, and case hardness is 21GPa, and bending strength is 918MPa, and fracture toughness is 5.26MPa m1/2, can meet the sintex instructions for use to performance.
Application Example 2
Al2O3The dispensing of base ceramic body, charging arrangement and microwave accept powder body with Application Example 1. Open after microwave, control the temperature of sintered specimen in two different heats in the time of about 50min and heat respectively and reached 1500 DEG C, 1700 DEG C, be incubated 10min subsequently. After having sintered, furnace cooling is to room temperature. Different heat sintered ceramic base substrates, along with increasing of most high sintering temperature, its consistency respectively 97.3% and 99.6%, case hardness is 18.6GPa and 22.3G respectively
A, bending strength is 880MPa and 950MPa respectively, and fracture toughness is 3.75MPa m1/2With 5.76MPa m1/2. Can meet the sintex instructions for use to performance.
Application Example 3
Al2O3The dispensing of base ceramic body, charging arrangement and microwave accept powder body with Application Example 1. The appropriate Cr adding trace2O3Powder accepts in powder body at inner core microwave. Opening after microwave, the temperature at the time sintered specimen of about 50min has just reached 1800 DEG C, is incubated 10min subsequently, and whole sintering process continues about about 60min, and after having sintered, furnace cooling is to room temperature. The relative density of obtained sintered specimen is 99.2%, and hardness is 21.6GPa, and bending strength is 900MPa, and fracture toughness is 4.26MPa m1/2, can meet the sintex instructions for use to performance.
In the various embodiments described above, microwave vacuum sintering furnace microwave frequency is 2.45GHz, when sintering, passes into the blanket of nitrogen of hydrogeneous 6%. Peak power output is 5KW. 6 magnetrons are respectively above and below microwave cavity, it is ensured that microwave field distribution is uniform. Infrared radiation thermometer can monitor sample temperature in resonator cavity in real time, and measured temperature ranges for 350 DEG C ~ 1800 DEG C.
As from the foregoing, assembly of the invention can bear relatively high sintering temperature, and uniformity of temperature profile, stable in addition with programming rate, good heat insulating, simple in construction, heating process is easily-controllable, feature with low cost, can be effectively improved production efficiency, the product comprehensive mechanical property simultaneously sintered is higher, meets the instructions for use of cutter material. Fully meet the requirement of microwave sintering attemperator, there is significantly high practical value.
Claims (9)
1. a microwave material placing device for high temperature sintering, is provided with microwave receptor powder bed inside described microwave material placing device, workpiece is placed in described microwave receptor powder bed and is sintered; It is characterized in that: described microwave receptor powder bed periphery is sequentially provided with internal layer heat-stable ceramic from the inside to the outside and builds film trap, outer layer heat-stable ceramic block film trap and heat-insulation layer; Described internal layer heat-stable ceramic builds film trap, outer layer heat-stable ceramic builds film trap and heat-insulation layer upper end open; It is filled with outer layer microwave between described internal layer heat-stable ceramic block film trap and outer layer heat-stable ceramic block film trap and accepts powder body; Described heat-insulation layer upper end open place is provided with outer layer insulation cover; Described outer layer insulation cover is provided with infrared measurement of temperature hole, is connected with microwave receptor powder bed.
2. microwave material placing device according to claim 1, it is characterised in that: described microwave receptor powder bed adopts inner core microwave to accept powder body; Described inner core microwave accepts powder body and adopts aluminium oxide, graphite and activated carbon with the volume ratio 70:15:15 mixed-powder formed; Described outer layer microwave accepts powder body and adopts carborundum, graphite and activated carbon with the volume ratio 60:20:20 mixed-powder formed.
3. microwave material placing device according to claim 2, it is characterised in that: described outer layer microwave accepts powder body and also includes the high lossy microwave material powder of trace; Described high microwave consume material is selected from Fe3O4��SnO2��MnO2Or Cr2O3; Described high lossy microwave material powder accounts for outer layer microwave and accepts the 1% of powder body gross weight.
4. microwave material placing device according to claim 2, it is characterised in that: described inner core microwave accepts powder body and outer layer microwave to accept the size of powder body be micron order.
5. according to the arbitrary described microwave material placing device of claims 1 to 3, it is characterised in that: described heat-insulation layer includes alumina fibre cotton layer, Alumina Foam brick layer and mullite casing from the inside to the outside successively; Described outer layer insulation cover adopts mullite lid.
6. microwave material placing device according to claim 5, it is characterised in that: described 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 all square, and upper end open.
7. microwave material placing device according to claim 6, it is characterised in that: described Alumina Foam brick layer upper end open place is provided with alumina fibre cotton lid; Described alumina fibre cotton lid is positioned at below described mullite lid; Described alumina fibre cotton covers and is provided with infrared measurement of temperature hole, and the infrared measurement of temperature hole that the infrared measurement of temperature hole on described mullite lid is covered by alumina fibre cotton is connected with described microwave receptor powder bed.
8. microwave material placing device according to claim 7, it is characterised in that: the pore size in described infrared measurement of temperature hole is 10mm.
9. according to the arbitrary described microwave material placing device of claims 1 to 3, it is characterised in that: described internal layer heat-stable ceramic builds film trap and outer layer heat-stable ceramic is built film trap and adopted aluminium oxide, boron nitride or nitrogenize staggered the piling up of silicon chip and form.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN107716927A (en) * | 2017-10-12 | 2018-02-23 | 钢铁研究总院 | A kind of identical temperature field multichannel honeycomb array crucible |
| CN108731475A (en) * | 2017-04-20 | 2018-11-02 | 南京理工大学 | A kind of ceramic material microwave sintering attemperator |
| CN110822899A (en) * | 2019-11-07 | 2020-02-21 | 南京理工大学 | Auxiliary heating and heat insulating device for microwave sintering |
| NL2032389A (en) * | 2021-07-12 | 2022-09-26 | Univ Zhengzhou | Energy-saving thermal insulation device for microwave kiln and method for preparing same |
| 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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| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
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| CN107716927A (en) * | 2017-10-12 | 2018-02-23 | 钢铁研究总院 | A kind of identical temperature field multichannel honeycomb array crucible |
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| CN110822899B (en) * | 2019-11-07 | 2021-03-02 | 南京理工大学 | Auxiliary heating and heat insulating device for microwave sintering |
| NL2032389A (en) * | 2021-07-12 | 2022-09-26 | Univ Zhengzhou | Energy-saving thermal insulation device for microwave kiln and method for preparing same |
| 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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