CN110579102A - ultra-high temperature sintering furnace and sintering method for oxide fiber product - Google Patents
ultra-high temperature sintering furnace and sintering method for oxide fiber product Download PDFInfo
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- CN110579102A CN110579102A CN201910743585.9A CN201910743585A CN110579102A CN 110579102 A CN110579102 A CN 110579102A CN 201910743585 A CN201910743585 A CN 201910743585A CN 110579102 A CN110579102 A CN 110579102A
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- 238000005245 sintering Methods 0.000 title claims abstract description 67
- 239000000835 fiber Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 23
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 108
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 93
- 239000010439 graphite Substances 0.000 claims abstract description 93
- 238000010438 heat treatment Methods 0.000 claims abstract description 50
- 238000002955 isolation Methods 0.000 claims abstract description 27
- 239000011241 protective layer Substances 0.000 claims abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 15
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 35
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 12
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 12
- 241001330002 Bambuseae Species 0.000 claims description 12
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 12
- 239000011425 bamboo Substances 0.000 claims description 12
- 229910026551 ZrC Inorganic materials 0.000 claims description 9
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims description 9
- 239000011094 fiberboard Substances 0.000 claims description 9
- 230000001681 protective effect Effects 0.000 claims description 8
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 238000005192 partition Methods 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- ZVWKZXLXHLZXLS-UHFFFAOYSA-N zirconium nitride Chemical compound [Zr]#N ZVWKZXLXHLZXLS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 206010037660 Pyrexia Diseases 0.000 claims description 2
- VWZIXVXBCBBRGP-UHFFFAOYSA-N boron;zirconium Chemical compound B#[Zr]#B VWZIXVXBCBBRGP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 23
- 239000007770 graphite material Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- 239000010410 layer Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000006229 carbon black Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 238000004380 ashing Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 238000002845 discoloration Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000002679 ablation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/04—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated adapted for treating the charge in vacuum or special atmosphere
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
- F27B5/08—Arrangements of linings
-
- 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
- F27D1/00—Casings; Linings; Walls; Roofs
- F27D1/0003—Linings or walls
- F27D1/0006—Linings or walls formed from bricks or layers with a particular composition or specific characteristics
-
- 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
- F27D5/00—Supports, screens, or the like for the charge within the furnace
- F27D5/0006—Composite supporting structures
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27M—INDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
- F27M2003/00—Type of treatment of the charge
- F27M2003/04—Sintering
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Tunnel Furnaces (AREA)
Abstract
the invention relates to an ultra-high temperature sintering furnace and a sintering method for oxide fiber products, the high temperature sintering furnace comprises a graphite electrode and a cylinder body, a hard felt cylinder is arranged in the cylinder body, a graphite felt and a carbon felt are arranged between the cylinder body and the hard felt cylinder, the graphite felt is close to one side of the hard felt cylinder, a graphite boat is arranged in the hard felt cylinder, a space is arranged between the graphite boat and the hard felt cylinder, a burning device is arranged in the graphite boat, and the graphite electrode is arranged in the space between the graphite boat and the hard felt cylinder. The high-temperature sintering furnace for the oxide fiber product adopts a graphite electrode as a heating mode, has a continuous or intermittent structure, and can be used in vacuum or N2And Ar and other inert gases are used for normal operation under the protection of high-efficiency, energy-saving and environment-friendly effects. The isolation protective layer is arranged, so that the graphite is not volatilized at high temperature, no reaction is caused between the graphite and the oxide, and no pollution is caused.
Description
Technical Field
The invention relates to an ultrahigh-temperature sintering furnace and a sintering method for an oxide fiber product, belonging to the technical field of high-temperature material heat treatment equipment.
background
The oxide fiber product is used as a material urgently needed by the aerospace and civil high-temperature heat-insulation, energy-saving and environment-friendly industries, and has the characteristics of high melting point, high temperature resistance, light weight, high strength and the like, such as ZrO2、MgO、Al2O3CaO and composite oxide fibers thereof, and the like, have very wide application and become a hotspot of research and development of various research institutions.
however, these oxides have very high melting points, above 2000 ℃, and have low viscosity at high temperature, so that it is difficult to prepare corresponding fiber materials by high-temperature melting methods, and sol-gel methods or polymer precursor methods are mostly adopted, and generally through processes such as spinning solution preparation, fiber formation, sintering and the like, and the diameter or volume of the fiber shrinks to different degrees as the treatment temperature of the fiber and its products rises. If the fiber product is not subjected to high-temperature treatment, the fiber product can continuously shrink in the using process, the original size and shape cannot be guaranteed, the energy-saving effect is reduced, and the material damage, the equipment ablation and even the personnel and property loss caused by high temperature are caused in serious cases.
The temperature of the high-temperature furnace which can be industrially used for a long time at present is up to 1700-1750 ℃, the temperature difference is hundreds of degrees from the melting point of the oxide, and the expected use temperature of the fiber material is 2000 ℃ or even higher. Therefore, the conventional high temperature furnace has not satisfied the actual demand. The temperature of 2000 ℃ or even 2300 ℃ can be reached by only two heating modes of graphite or tungsten and molybdenum, wherein the tungsten and molybdenum are heated to reach the limit of temperature and are difficult to reuse, and the volatilization at high temperature is serious, so that the product is polluted, and the cost is high. The graphite heating mode has large and adjustable temperature space, and can be made into continuous or intermittent high temperature furnace in vacuum or N2And Ar and other inert gases can normally operate under the protection of inert gases, but the most main problem is that graphite volatilizes or contacts Al at high temperature2O3、ZrO2The oxides such as MgO and the like react, and C is combined with O in the oxides, so that the loss and damage of the graphite plate or the heating element are caused, and the service life of the equipment is reduced; secondly, a large amount of CO is formed, which causes pollution to the environment and products.
In addition, chinese patent document CN1352375A discloses a resistance heating type ultra-high temperature vacuum sintering furnace, which mainly includes a furnace body, a resistance heating device, and auxiliary devices such as a vacuum pressure and ultra-high temperature detection part; two poles of a power supply in the resistance heating device enter the sintering furnace through a large-current bus outside the furnace and a metal water-cooling electrode, and are connected to a heating body plate frame through a transition electrode made of a carbon-graphite material to form a complete loop system; the heating body plate frame in the resistance heating device adopts a circuit structure that the upper heating body and the lower heating body on one side are connected in series and the two sides are connected in parallel. Chinese patent document CN100347507C discloses a sintering furnace for preparing zirconia continuous fibers, which is characterized by mainly comprising an inner tube and an outer tube, wherein the inner tube and the outer tube are both made of quartz or alumina, zirconia ceramics, the outer tube is used for heating, and heating furnace wires are uniformly wound outside the outer tube; the inner pipe is used for blowing, one end of the inner pipe is closed, the other end of the inner pipe is communicated with the outside, a gas valve is connected to the inner pipe, slits are evenly carved on the inner pipe along the circumference of the inner pipe wall in the axial direction, airflow can be blown out of the inner pipe in a radial mode through the small slits during ventilation, the inner pipe is sleeved in the outer pipe, the circumference of the outer pipe is wrapped with a heat insulation layer, the two ends of the outer pipe are plugged with closed heat insulation ceramic plugs, the inner pipe and the outer pipe are sleeved together through a plug at one end, a quartz or ceramic pipe which is directly communicated with the outside, has the same diameter as the inner pipe and is. The sintering furnace is complex in structure, components of the sintering furnace are not processed, and reaction between graphite and oxide fibers cannot be avoided in the high-temperature sintering process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the ultrahigh-temperature sintering furnace and the sintering method for the oxide fiber product, the sintering furnace can prevent the reaction between graphite and the processed oxide fiber so as to obtain the oxide fiber product subjected to ultrahigh-temperature processing, and simultaneously prevent the oxidation of a furnace body and internal accessories, prolong the service life and reduce the environmental pollution.
The technical scheme of the invention is as follows:
The utility model provides an ultra-high temperature fritting furnace for oxide fiber product, includes graphite electrode and barrel, the barrel in be provided with hard felt section of thick bamboo, barrel and hard felt section of thick bamboo between be provided with graphite felt and carbon felt, the graphite felt be close to one side of hard felt section of thick bamboo, hard felt section of thick bamboo in be provided with the graphite boat, graphite boat and hard felt section of thick bamboo between be provided with the interval, the graphite boat in be provided with and hold the fever device, the graphite electrode sets up in the interval between graphite boat and hard felt section of thick bamboo.
According to the invention, the graphite boat is preferably of a cavity structure and made of graphite materials, and the left side and the right side of the inner wall of the cavity are respectively provided with a protrusion. The inner space of the graphite boat is divided into a plurality of layers by the arrangement of the protrusions, so that the space of a hearth can be fully utilized, and the sintering efficiency is improved. The protrusions of different levels can bear multiple layers of burning bearing plates. During the use process, the graphite boat can be sealed if necessary to form a temperature field with uniform temperature.
According to the invention, preferably, the inner wall of the graphite boat is provided with an isolation protective layer for preventing graphite from volatilizing at high temperatureand (4) sending. The preferable isolation protective layer is made of BN or SiO2、SiC、ZrB2And the like, are high temperature resistant, oxidation resistant, insulating and heat conducting materials.
According to the invention, preferably, vent holes are arranged below the graphite boat and the hard felt cylinder and used for introducing N2And inert gases such as Ar and the like can effectively reduce the useless components generated in the sintering process.
According to the invention, preferably, the hard felt cylinder is of a cavity structure and is made of graphite; the graphite felt and the carbon felt surround the hard felt cylinder. The graphite felt, the carbon felt and the hard felt cylinder jointly form a heat preservation layer of the sintering furnace, and the heat preservation, heat insulation and energy saving effects are optimal. The graphite felt is obtained by treating the carbon felt at the high temperature of 1800 plus 2000 ℃. The hard felt cylinder and the graphite felt made of graphite can endure the high temperature of more than 2000 ℃, and provide sufficient heat preservation effect for the sintering furnace.
according to the invention, preferably, the burning device comprises a first burning board, the upper surface of the first burning board is provided with a groove, a burning ball is arranged in the groove, and the burning ball protrudes out of the surface of the first burning board and can rotate in the groove.
The first burning bearing plate is provided with a groove, and a burning bearing ball is arranged in the groove. The arrangement greatly reduces the contact area between the oxide fiber board and the first burning bearing board, and reduces the friction resistance when the oxide fiber board shrinks. Meanwhile, the burning ball can rotate in the groove, so that the frictional resistance of the oxide fiber board is further reduced.
According to the invention, the diameter of the groove is preferably larger than that of the burning ball, and the diameter of the burning ball is more preferably 5-10 mm. The arrangement is more beneficial to the burning ball to rotate in the groove.
According to the invention, preferably, the grooves are hemispherical grooves which are uniformly distributed on the surface of the first burning bearing plate; further preferably, the distance between the centers of two adjacent grooves is 20-30 mm.
According to the present invention, preferably, the burning equipment is further provided with two or more second burning bearing plates supported by the burning bearing balls, and the area of the second burning bearing plates is smaller than that of the first burning bearing plates.
According to the present invention, preferably, the second setter plate has a square or circular shape. Further preferably, the size of the square second burning board is (70-100) × (50-70) × (5-10) mm, and the diameter of the round second burning board is 30-100mm and the thickness is 5-10 mm.
According to the invention, preferably, a space is arranged between two adjacent second burning bearing plates, and further preferably, the space is 15-30 mm. The second setter plate can further bear the oxide fiber plate, and when the oxide fiber plate shrinks, the second setter plate can slide on the setter ball, so that the oxide fiber plate is further prevented from being broken due to uneven shrinkage. And a space is arranged between the second burning bearing plates, so that enough space is reserved between the second burning bearing plates when the oxide fiber plate shrinks at high temperature.
According to the present invention, preferably, the first burning plate, the burning ball and the second burning plate are made of graphite. The graphite material can realize heat treatment at higher temperature. Further preferably, a partition plate is further arranged above the second burning bearing plate. The size and the spacing between the isolation plates are the same as those of the second burning bearing plate. Preferably, the material used for the isolation plate has high-temperature strength and stability and good thermal conductivity, such as one of zirconium boride, zirconium carbide, zirconium nitride and the like or a mixture thereof. When the second sintering plate is in a working state, the isolation plate is positioned between the second sintering plate and the oxide fiber plate, so that the second sintering plate made of graphite can be prevented from being in direct contact with the oxide fiber plate, and chemical reaction between the second sintering plate and the oxide fiber plate is avoided.
According to the invention, the sintering method for the oxide fiber product by using the ultrahigh-temperature sintering furnace comprises the following steps:
(1) After the oxide fiber board to be sintered is arranged, the temperature of the ultra-high temperature sintering furnace is raised, wherein the temperature raising procedure is as follows: heating to 600 ℃ for 4h, then heating to 1500 ℃ for 5h, and heating to 1800 ℃ for 2 h; heating to 1950 ℃ within 2h, keeping the temperature at 1950 ℃ for 2h, and then cooling; cooling to 1700 ℃ in 100min, 1500 ℃ in 60min, and then naturally cooling to room temperature;
Or heating to 600 ℃ within 4h, then heating to 1500 ℃ within 5h, and heating to 1800 ℃ within 2 h; heating to 2000 ℃ for 3h, keeping the temperature at 2000 ℃ for 2h, and then cooling; cooling to 1400 ℃ within 200min, and then naturally cooling to room temperature;
Or heating to 600 ℃ within 4h, then heating to 1500 ℃ within 5h, and heating to 1800 ℃ within 2 h; heating to 2050 ℃ within 200min, keeping the temperature of 2050 ℃ for 2h, and then cooling; cooling to 1500 ℃ within 200min, and then naturally cooling to room temperature;
or heating to 600 ℃ within 4h, then heating to 1500 ℃ within 5h, and heating to 1800 ℃ within 2 h; heating to 2200 ℃ after 4h, keeping the temperature at 2200 ℃ for 3h, and then cooling; cooling to 1500 ℃ in 300min, and then naturally cooling to room temperature;
(2) The gas environment in the sintering process is as follows: before the temperature is raised to 600 ℃, the furnace is kept vacuumized, and the vacuum degree is-0.1 MPa; n is used before cooling to 1500 DEG C2making protective atmosphere, and then keeping vacuumizing until the temperature is reduced to 600 ℃, wherein the vacuum degree is-0.1 MPa;
Or N is used after the temperature is increased to 600 ℃ and before the temperature is reduced to 1500 DEG C2Making a protective atmosphere, and keeping vacuumizing at the vacuum degree of-0.1 MPa at other times;
The invention has not been described in detail, but is in accordance with the state of the art.
The invention has the following characteristics and beneficial effects:
1. The high-temperature sintering furnace for the oxide fiber product adopts a graphite electrode as a heating mode, has a continuous or intermittent structure, and can be used in vacuum or N2And Ar and other inert gases are used for normal operation under the protection of high-efficiency, energy-saving and environment-friendly effects. The isolation protective layer is arranged, so that the graphite is not volatilized at high temperature, no reaction is caused between the graphite and the oxide, and no pollution is caused.
2. In the burning device, the first burning board is provided with the groove, and the burning ball is arranged in the groove, so that the contact area between the oxide fiber board and the first burning board is greatly reduced, and the friction resistance when the oxide fiber board contracts is reduced. Meanwhile, the burning ball can rotate in the groove, so that the frictional resistance of the oxide fiber board is further reduced. The second setter plate can further bear the oxide fiber plate, and when the oxide fiber plate shrinks, the second setter plate can slide on the setter ball, so that the oxide fiber plate is further prevented from being broken due to uneven shrinkage. Meanwhile, the isolation plate is arranged above the second burning bearing plate, so that the second burning bearing plate made of graphite can be prevented from being in direct contact with the oxide fiber plate, and chemical reaction between the second burning bearing plate and the oxide fiber plate is avoided.
3. By using the sintering furnace, the oxide fiber product is well-retained and regular in size after being sintered at high temperature, and has the characteristics of no shrinkage, no deformation and no pollution within the range of 1700-2200 ℃.
Description of the drawings:
FIG. 1 is a schematic view of the main structure of the ultra-high temperature sintering furnace of the present invention.
FIG. 2 is a schematic structural diagram of a main body of a graphite boat in a hard felt cylinder of the ultra-high temperature sintering furnace.
FIG. 3 is a schematic structural diagram of a main body of the load bearing device in the ultra-high temperature sintering furnace of the invention.
Wherein: 1. a stiff felt cylinder; 2. a barrel; 3. graphite felt; 4. a carbon felt; 5. the device comprises a burning device, 5-1 parts of a first burning board, 5-2 parts of a burning ball, 5-3 parts of a second burning board, 5-4 parts of an isolation board, 5-5 parts of a groove; 6. a graphite boat; 7. and (8) vent holes, and an oxide fiber plate.
The specific embodiment is as follows:
The present invention will be further described with reference to the following examples, but is not limited thereto, in conjunction with the accompanying drawings.
Example 1
As shown in fig. 1-3, an ultra-high temperature sintering furnace for oxide fiber products comprises a graphite electrode and a cylinder body 2, the cylinder body 2 is internally provided with a hard felt cylinder 1, the cylinder body 2 and the hard felt cylinder 1 are provided with a graphite felt 3 and a carbon felt 4 therebetween, the graphite felt 3 is close to one side of the hard felt cylinder 1, the hard felt cylinder 1 is internally provided with a graphite boat 6, the graphite boat 6 and the hard felt cylinder 1 are arranged at intervals, the graphite boat 6 is internally provided with a burning device 5, and the graphite electrode is arranged at intervals between the graphite boat 6 and the hard felt cylinder 1.
the graphite boat 6 is of a cavity structure and is made of graphite materials, and the left side and the right side of the inner wall of the cavity are respectively provided with a bulge. The inner space of the graphite boat 6 is divided into a plurality of layers by the arrangement of the protrusions, so that the space of a hearth can be fully utilized, and the sintering efficiency is improved. The different levels of protuberances can carry multiple layers of setter plates 5.
The inner wall of the graphite boat 6 is provided with an isolation protective layer for preventing graphite from volatilizing at high temperature. The isolation protective layer is made of BN or SiO2SiC or ZrB2。
The lower part of the graphite boat 6 and the lower part of the hard felt cylinder 1 are provided with vent holes 7 for introducing N2and inert gases such as Ar and the like can effectively reduce the useless components generated in the sintering process.
the hard felt cylinder 1 is of a cavity structure and is made of graphite; the graphite felt 3 and the carbon felt 4 surround the hard felt cylinder 1. The graphite felt 3, the carbon felt 4 and the hard felt cylinder 1 jointly form a heat preservation layer of the sintering furnace, and the heat preservation, heat insulation and energy saving effects are optimal. The graphite felt 3 is obtained by treating the carbon felt 4 at the high temperature of 1800 plus 2000 ℃. The hard felt cylinder 1 and the graphite felt 3 made of graphite materials can bear the high temperature of more than 2000 ℃, and provide a sufficient heat preservation effect for the sintering furnace.
the burning device 5 comprises a first burning plate 5-1, a groove 5-5 is formed in the upper surface of the first burning plate 5-1, a burning ball 5-2 is arranged in the groove 5-5, and the burning ball 5-2 protrudes out of the surface of the first burning plate 5-1 and can rotate in the groove 5-5. The diameter of the groove 5-5 is larger than that of the burning ball 5-2, and the diameter of the burning ball 5-2 is 5-10 mm. The grooves 5-5 are hemispherical grooves, and the grooves 5-5 are uniformly distributed on the surface of the first burning bearing plate 5-1; the center distance between two adjacent grooves 5-5 is 20-30 mm. The burning device 5 is also provided with more than two second burning bearing plates 5-3 and is supported by the burning bearing balls 5-2, and the area of the second burning bearing plates 5-3 is smaller than that of the first burning bearing plates 5-1. The second burning bearing plate 5-3 is square or round. The size of the square second burning bearing plate 5-3 is (70-100) × (50-70) × (5-10) mm, and the diameter of the round second burning bearing plate 5-3 is 30-100mm and the thickness is 5-10 mm. And a space is arranged between every two adjacent second burning bearing plates 5-3, and the size of the space is 15-30 mm. The first burning bearing plate 5-1, the burning bearing balls 5-2 and the second burning bearing plate 5-3 are made of graphite materials. An isolation plate 5-4 is also arranged above the second burning bearing plate 5-3. The size and the interval between the insulation plates 5-4 are the same as those of the second setter plates 5-3. The material used for the isolation plates 5-4 has high-temperature strength and stability and good thermal conductivity, such as one of zirconium boride, zirconium carbide, zirconium nitride and the like or a mixture of the zirconium boride, the zirconium carbide and the zirconium nitride.
Example 2
As described in example 1, except that:
The protective layer on the inner wall of the graphite boat 6 is SiC for placing products to be sintered, the first sintering bearing plate 5-1 is a graphite sintering bearing plate with 420 x 320 x 30mm, and the isolation plate 5-4 adopts ZrB with 70 x 50 x 10mm2The blocks were arranged, on which were placed a block size of 400 x 300 x 60mm and a density of 0.4g/cm3the zirconia fiber sheet of (1). The operations are repeated to manufacture six groups of samples to be sintered, then the six groups of samples are placed in the graphite boat 6, and the front door and the rear door of the sintering furnace are sealed (temperature measuring holes are reserved on the doors).
After the arrangement is finished, the ultrahigh-temperature sintering furnace is heated up to 600 ℃ in 4 hours, then heated up to 1500 ℃ in 5 hours, heated up to 1800 ℃ in 2 hours, heated up to 1950 ℃ in 2 hours, and kept at 1950 ℃ for 2 hours, and then the temperature is reduced. Cooling to 1700 ℃ in 100min, 1500 ℃ in 60min, and then naturally cooling to room temperature.
The gas environment in the sintering process is as follows: before the temperature is raised to 600 ℃, the furnace is kept vacuumized, and the vacuum degree is-0.1 MPa. N is used before the temperature is reduced to 15002Making protective atmosphere, then reducing to 600 deg.C, and maintaining vacuum degree of-0.1 MPa.
The ashless and crack-free zirconium oxide sample is obtained after the furnace is opened, and the average density is measured to be 0.64g/cm3. The inner wall of the graphite boat 6 is touched by hands, and no obvious carbon black phenomenon exists; and the isolation protective layer is still intact when the inner wall is observed. Observation of ZrB2The contact surface of the isolation plate 5-4 and the carbon plate has no reaction phenomena of color change and the like, ZrB2The isolation plates 5-4 are kept complete without cracking and can be repeatedly used.
Example 3
As described in example 1, except that:
The protective layer of the inner wall of the graphite boat 6 is SiC for placing products to be burnt. The first setter plate 5-1 is a graphite setter plate of 420 x 320 x 30, the isolation plates 5-4 are arranged by using ZrN blocks of 70 x 50 x 10mm, and three groups of upper setting rulers are arrangedInch of 400 × 300 × 60mm, and density of 0.3g/cm3the other three groups of the zirconia fiber boards are placed on the same size and density of 0.4g/cm3The zirconia fiber sheet of (1). Six groups of samples were placed in a graphite boat 6, and front and rear doors were sealed.
After the arrangement is finished, the ultra-high temperature sintering furnace is heated up, wherein the temperature is raised to 600 ℃ in 4h, then to 1500 ℃ in 5h, to 1800 ℃ in 2h, to 2000 ℃ in 3h, and the temperature is kept at 2000 ℃ for 2h, and then the temperature is lowered. Cooling to 1400 ℃ in 200min, and then naturally cooling to room temperature.
The gas environment in the sintering process is as follows: n is used after the temperature is increased to 600 ℃ and before the temperature is reduced to 1400 DEG C2And (5) making a protective atmosphere, and keeping vacuumizing at the vacuum degree of-0.1 MPa at other times.
Obtaining a non-ashing and non-crack zirconia sample after opening the furnace, and measuring the density change condition to be 0.3g/cm3It became 0.55g/cm3；0.4g/cm3it became 0.65g/cm3. The inner wall of the graphite boat 6 is touched by hands, and no obvious carbon black phenomenon exists; and the isolation protective layer is still intact when the inner wall is observed. And observing that the contact surface of the ZrN isolating plate 5-4 and the carbon plate has no reaction phenomena such as discoloration and the like, wherein most of the ZrN isolating plate 5-4 is kept intact without cracking and can be repeatedly used.
Example 4
As described in example 1, except that:
The protective layer of the inner wall of the graphite boat 6 is BN for placing products to be burnt, the first burning bearing plate 5-1 is a graphite burning bearing plate with 420 x 320 x 30mm, three groups of isolation plates 5-4 are arranged by ZrN blocks with 70 x 50 x 10mm, and the other three groups are arranged by ZrB blocks with the same size2Arranging two blocks with size of 300 × 200 × 60mm and density of 0.5g/cm3The zirconia fiber sheet of (1). Six groups of samples were placed in a graphite boat 6, and front and rear doors were sealed.
After the arrangement is finished, the ultra-high temperature sintering furnace is heated up, wherein the temperature is raised to 600 ℃ within 4h, then to 1500 ℃ within 5h, to 1800 ℃ within 2h, to 2050 ℃ within 200min, and the temperature of 2050 ℃ is kept constant for 2h, and then the temperature is lowered. Cooling to 1500 ℃ in 200min, and then naturally cooling to room temperature.
the gas environment in the sintering process is as follows: after heating to 600 deg.C toN is used before the temperature is reduced to 15002And (5) making a protective atmosphere, and keeping vacuumizing at the vacuum degree of-0.1 MPa at other times.
Obtaining a non-ashing and non-crack zirconia sample after opening the furnace, and measuring the average density of the sample to be 1.0g/cm3. The inner wall of the graphite boat 6 is touched by hands, and no obvious carbon black phenomenon exists; and the inner wall is observed, and the isolation protective layer is intact. ZrN/ZrB2the contact surface of the isolation plate 5-4 and the carbon plate has no reaction phenomena of discoloration and the like, ZrN/ZrB2The isolation plates 5-4 are kept complete without cracking and can be repeatedly used.
example 5
As described in example 1, except that:
The protective layer on the inner wall of the graphite boat 6 is SiC, the first sintering bearing plate 5-1 is a graphite sintering bearing plate with 420X 320X 30mm, the isolation plate 5-4 is arranged by adopting ZrC blocks with 70X 50X 10mm, and two ZrC blocks with the size of 400X 150X 60mm and the density of 1.0g/cm are placed on the ZrC blocks3The zirconia fiber sheet of (1). The above operations are repeated to make six groups of samples to be burned, and then the six groups of samples are placed in the graphite boat 6, and the front door and the rear door are sealed.
After the arrangement is finished, the ultra-high temperature sintering furnace is heated up, wherein the temperature is raised to 600 ℃ within 4h, then to 1500 ℃ within 5h, to 1800 ℃ within 2h, to 2200 ℃ within 4h, and then to 2200 ℃ within 2200 ℃ for 3h, and then the temperature is reduced. And cooling to 1500 ℃ in 300min, and then naturally cooling to room temperature.
The gas environment in the sintering process is as follows: n is used after the temperature is increased to 600 ℃ and before the temperature is reduced to 1500 DEG C2And (5) making a protective atmosphere, and keeping vacuumizing at the vacuum degree of-0.1 MPa at other times.
Obtaining a non-ashing and non-crack zirconia sample after opening the furnace, and measuring that the average density is 1.65g/cm3. The inner wall of the graphite boat 6 is touched by hands, and no obvious carbon black phenomenon exists; and the isolation protective layer is still intact when the inner wall is observed. The ZrC separating plate 5-4 has no reaction phenomena such as discoloration and the like with the contact surface of the carbon plate, and the ZrC separating plate 5-4 is kept complete without cracking and can be repeatedly used.
Claims (10)
1. The utility model provides an ultra-high temperature fritting furnace for oxide fiber product, includes graphite electrode and barrel, its characterized in that, the barrel in be provided with hard felt section of thick bamboo, barrel and hard felt section of thick bamboo between be provided with graphite felt and carbon felt, the graphite felt be close to one side of hard felt section of thick bamboo, hard felt section of thick bamboo in be provided with the graphite boat, graphite boat and hard felt section of thick bamboo between be provided with the interval, the graphite boat in be provided with and hold the fever device, the graphite electrode sets up in the interval between graphite boat and hard felt section of thick bamboo.
2. The ultra-high temperature sintering furnace according to claim 1, wherein the graphite boat is of a cavity structure and is made of graphite, and the left side and the right side of the inner wall of the cavity are respectively provided with a protrusion.
3. The ultra-high temperature sintering furnace according to claim 1, wherein the inner wall of the graphite boat is provided with an isolation protective layer for preventing graphite from volatilizing at high temperature; the preferable isolation protective layer is made of BN or SiO2SiC or ZrB2。
4. the ultra-high temperature sintering furnace according to claim 1, wherein vent holes are arranged below the graphite boat and the hard felt cylinder for introducing inert gas.
5. The ultra-high temperature sintering furnace according to claim 1, wherein the burning bearing device comprises a first burning bearing plate, a groove is arranged on the upper surface of the first burning bearing plate, a burning bearing ball is arranged in the groove, and the burning bearing ball protrudes out of the surface of the first burning bearing plate and can rotate in the groove.
6. The ultra-high temperature sintering furnace according to claim 5, wherein the diameter of the groove is larger than that of the burning ball, and the diameter of the burning ball is 5-10 mm.
7. The ultrahigh-temperature sintering furnace according to claim 5, wherein the grooves are hemispherical grooves, and the grooves are uniformly distributed on the surface of the first burning bearing plate; preferably, the distance between the centers of two adjacent grooves is 20-30 mm.
8. The ultra-high temperature sintering furnace according to claim 5, wherein the burning bearing device is further provided with more than two second burning bearing plates and supported by the burning bearing balls, and the area of the second burning bearing plates is smaller than that of the first burning bearing plates.
9. the ultrahigh-temperature sintering furnace according to claim 5, wherein a space is arranged between two adjacent second burning bearing plates;
Preferably, the second setter plate is further provided with a partition plate above, the size and the interval between the partition plates are the same as those of the second setter plate, and the partition plate is made of zirconium boride, zirconium carbide or zirconium nitride.
10. A sintering method for an oxide fiber product using the ultra-high temperature sintering furnace as claimed in any one of claims 1 to 9, comprising the steps of:
(1) After the oxide fiber board to be sintered is arranged, the temperature of the ultra-high temperature sintering furnace is raised, wherein the temperature raising procedure is as follows: heating to 600 ℃ for 4h, then heating to 1500 ℃ for 5h, and heating to 1800 ℃ for 2 h; heating to 1950 ℃ within 2h, keeping the temperature at 1950 ℃ for 2h, and then cooling; cooling to 1700 ℃ in 100min, 1500 ℃ in 60min, and then naturally cooling to room temperature;
Or heating to 600 ℃ within 4h, then heating to 1500 ℃ within 5h, and heating to 1800 ℃ within 2 h; heating to 2000 ℃ for 3h, keeping the temperature at 2000 ℃ for 2h, and then cooling; cooling to 1400 ℃ within 200min, and then naturally cooling to room temperature;
Or heating to 600 ℃ within 4h, then heating to 1500 ℃ within 5h, and heating to 1800 ℃ within 2 h; heating to 2050 ℃ within 200min, keeping the temperature of 2050 ℃ for 2h, and then cooling; cooling to 1500 ℃ within 200min, and then naturally cooling to room temperature;
Or heating to 600 ℃ within 4h, then heating to 1500 ℃ within 5h, and heating to 1800 ℃ within 2 h; heating to 2200 ℃ after 4h, keeping the temperature at 2200 ℃ for 3h, and then cooling; cooling to 1500 ℃ in 300min, and then naturally cooling to room temperature;
(2) The gas environment in the sintering process is as follows: before the temperature is raised to 600 ℃, the temperature in the furnace is keptVacuum pumping is kept, and the vacuum degree is-0.1 MPa; n is used before cooling to 1500 DEG C2making protective atmosphere, and then keeping vacuumizing until the temperature is reduced to 600 ℃, wherein the vacuum degree is-0.1 MPa;
Or N is used after the temperature is increased to 600 ℃ and before the temperature is reduced to 1500 DEG C2And (5) making a protective atmosphere, and keeping vacuumizing at the vacuum degree of-0.1 Mpa for other times.
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Application publication date: 20191217 |