CN101050121A - Dual heating mode flash sintering method combining current heating with radiant heating - Google Patents
Dual heating mode flash sintering method combining current heating with radiant heating Download PDFInfo
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- CN101050121A CN101050121A CN 200710051776 CN200710051776A CN101050121A CN 101050121 A CN101050121 A CN 101050121A CN 200710051776 CN200710051776 CN 200710051776 CN 200710051776 A CN200710051776 A CN 200710051776A CN 101050121 A CN101050121 A CN 101050121A
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Abstract
This invention relates to a method for preparing block material from powdery material by sintering. The method is a rapid sintering method by combination of electric heating and radiation heating. The electricity/radiation power ratio is (5-30):1. The radiation heater/mold height ratio is (1-3):2. Samples with diameters greater than 30 mm are heated through combination of electric heating and radiation heating at a heating rate of 100-800 deg.C/min; the heat preservation time is 3-15 min. After heat preservation, electric heating and radiation heating terminated, and the samples are naturally cooled. The method can be used to prepare samples with uniform inner structure and diameters greater than 30 mm, and has such advantages as short sintering time and low energy consumption.
Description
Technical field
The present invention relates to a kind ofly be prepared into the sintering method of block materials, particularly relate to the flash sintering method of the closely knit block materials of preparation (comprising pottery, ceramic matric composite, metal, metal-base composites, ceramic/metal composite materials etc.) by powdered material.
Background technology
The most effective preparation method of block materials such as pottery and ceramic matric composite is that preparation, moulding, sintering and the following process by raw material powder finished, and sintering process is a step the most key in the whole preparation method, and it has determined the final performance of prepared material to a great extent.Along with the raw material powder Development of Preparation Technology, people have obtained the ultrafine powder of a large amount of excellent performances, wish to prepare the same excellent block materials of performance, and the focus of the whole process of material preparation has focused on the sintering process of material.
The sintering of powdered material has several different methods, sintering method commonly used has 1. pressureless sintering, 2. gas pressure sintering, 3. hot pressed sintering, 4. HIP sintering, 5. microwave sintering, 6. electric current (comprising pulse, direct current, alternating current) sintering etc., each sintering method characteristic is obvious: 1., 2. two kinds of methods are difficult to obtain compact material owing to can not directly exert pressure to sample to most of novel materials; 3., 4. two kinds of methods can obtain closely knit block materials, but sintering time is long, power consumption is high, cost is high; 5., 6. two kinds of method quick heatings, but prepare block materials within a short period of time, but microwave sintering is difficult to exert pressure when heating up, be difficult for obtaining fine and close fully material, also exist uniform temperature zone less simultaneously, can not prepare the weakness of even structure large size sample, the electric current sintering method then can apply certain mechanical force when being rapidly heated, obtain fine and close block materials easily, therefore more and more be widely used.
The electric current sintering method is widely used at aspects such as preparation pottery, ceramic composite, metal, metal/ceramic composite, prepared the block materials of many excellent performances, but increasing user finds to exist when this method prepares block materials a fatal weakness: when the block materials diameter of preparation surpasses 30mm, occur the non-uniform phenomenon of material internal structure in the sample inevitably.
Summary of the invention
The object of the present invention is to provide the dual heating mode flash sintering method of a kind of current flow heats in conjunction with radiation heating, this method can be prepared the sample (be block materials) of the diameter of material internal even structure greater than 30mm, and sintering time is short, energy-conservation.
To achieve these goals, technical scheme of the present invention is: a kind of current flow heats is in conjunction with the dual heating mode flash sintering method of radiation heating, it is characterized in that in electric current sintering equipment, disposing radiant heating device than 30: 1～5: 1 by current flow heats power and radiation heating power, the radiation heating heating element installation site of radiant heating device is between the chamber wall of the mould outside and electric current sintering equipment, and radiation heating heating element height and mold height were with 1: 2～3: 2 couplings; At the sintering diameter during greater than the sample of 30mm, adopt Fast Sintering under current flow heats and the radiation heating dual heating mode, mold surface temperature and radiation heating heating element temperature gap be controlled at mold surface temperature 15% in, temperature rise rate is controlled at 100～800 ℃/min in the temperature-rise period, and soaking time is controlled at 3～15min; When the sintering diameter is less than or equal to the sample of 30mm, adopt Fast Sintering under current flow heats and the radiation heating dual heating mode, mold surface temperature and radiation heating heating element temperature gap be controlled at mold surface temperature 15% in, temperature rise rate can be controlled in 800～1000 ℃/min in the temperature-rise period, soaking time is controlled at 0～3min, is beneficial to the thin brilliant closely knit block materials of sintering; Insulation finishes the power supply that the back cuts off current flow heats and radiation heating, naturally cooling.
Described radiant heating device has and overlaps independently power supply and supply with and temperature measuring system.When radiant heating device works independently (power supply of electric current sintering equipment disconnects), the radiant heating device working order is similar to a hot pressing furnace, can finish the hot pressing furnace repertoire; When electric current sintering equipment works independently (power supply that is radiant heating device disconnects), can carry out the electric current Fast Sintering that diameter is less than or equal to the 30mm sample, obtain closely knit block materials; When electric current sintering equipment and radiant heating device are opened simultaneously and are entered matching status, can carry out the electric current Fast Sintering of diameter greater than the 30mm sample, obtain the closely knit block materials of diameter greater than the even structure of 30mm.
Described radiation heating heating element is that forms such as shape are installed in round shape, square tube shape or dispersion, and radiation heating heating element material is a graphite.
1-10 floor height temperature thermofin is set between the chamber wall of described radiation heating heating element and electric current sintering equipment, and high temperature insulating layer material is carbon fiber felt.
Described sample is stupalith, ceramic matric composite (comprising matrix materials such as pottery/pottery, ceramic/metal), metal or metal-base composites.
Find through years of researches, prepare in the process of block materials at electric current sintering, from the sample center to sample edge, the mould inboard all exists temperature difference phenomenon to the mould outer rim, the sample core temperature is higher than the sample edge temperature, and the big more sintering temperature of sample size is high more, the temperature difference is big more, the existence of temperature difference phenomenon directly has influence on the formation of sample interior structural inhomogeneity, the instability of performance when causing the electric current sintering diameter greater than the 30mm sample has limited this electric current sintering preparation method's broader applications.As sintering TiB2-BN complex phase ceramic, sintering condition is 3 ℃/S of temperature rise rate, 1800 ℃ of sintering temperatures, sample size φ 50 * 10mm
2, the radial direction temperature difference between sample center and the sample edge surpasses 400 ℃, is the closely knit block materials that impossible obtain even structure under this temperature field condition.The present invention is further developing on electric current sintering method basis, by the one cover radiant heating device of coupling in electric current sintering equipment, the compound heating mode that adopts current flow heats and two kinds of heating modes of radiation heating to work simultaneously, it inherited electric current sintering method Fast Sintering advantage (temperature rise rate can reach 800 ℃/min), changed the temperature distributing rule in the sintering process simultaneously, realized the dense samples of the diameter of preparation even structure, and sintering time is short, energy-conservation greater than 30mm; Two cover heating modes respectively have clear and definite purpose: heating mode 1---current flow heats realizes being rapidly heated, heating mode 2---radiation heating is realized samming, improve the radial temperature profile in sintered sample and the mould, the radial temperature profile in sample particularly, obtain uniform temperature field (sample area highest temperature difference is less than 50 ℃), thereby provide effective guarantee for the block materials of preparation even structure.
Compare with electric current (comprise pulse, direct current, the exchange) sintering method of routine, the present invention is with the obvious advantage during greater than the sample of 30mm at the sintering diameter, and the electric current sintering system of band radiant heating device can prepare the sample of the diameter of material internal even structure greater than 30mm; Such sintering system is compared with the same hot-pressing sintering method that can prepare the large size sample then in that to shorten aspect sintering time and the energy-saving effect advantage fairly obvious; With preparation φ 100 * 10mm
2Sample be example, compare with hot-pressing sintering method, this method (temperature-rise period is less than 10min) is at short notice finished preparation, the band radiation heating the electric current sintering method can save energy more than 40%, the heating-up time is less than 1/10 of hot-pressing sintering method.Adopt sintering method provided by the invention can not only prepare pottery, ceramic matric composite, also can prepare metal, metal-base composites and metal/ceramic composite, purposes is very extensive, and great practical extending application value is arranged.
Description of drawings
Fig. 1 is the structural representation of electric current sintering system of realizing the band radiant heating device of the inventive method
Fig. 2 is the sectional view of Fig. 1 along the A-A line
Fig. 3 is the structural representation of radiation heating heating element
Fig. 4 is the vertical view of Fig. 3
Fig. 5 is alumina sample scanning electronic microscope (SEM) photo
Fig. 6 is alumina sample transmission electron microscope (TEM) photo
Among the figure: 1---sample, 2---mould, 3---the radiation heating heating element, 4---the chamber wall of electric current sintering equipment.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
A kind of current flow heats is in conjunction with the dual heating mode flash sintering method of radiation heating, and 1, at first in electric current sintering equipment, disposed radiant heating device (as shown in Figure 1 and Figure 2) than 5: 1 by current flow heats power and radiation heating power; Radiation heating heating element 3 installation sites of radiant heating device are between the chamber wall 4 of mould 2 outsides and electric current sintering equipment, 10 floor height temperature thermofins are set between the chamber wall of described radiation heating heating element and electric current sintering equipment, and high temperature insulating layer material is carbon fiber felt; Radiation heating heating element height and mold height were with 1: 2 coupling, and the radiation heating heating element is a square tube shape, and radiant heating device has and overlaps independently power supply and supply with and temperature measuring system.
2, the flash sintering method of current flow heats and radiation heating dual heating mode prepares TiB
2-BN complex phase ceramic (sample 1) will mix the TiB that proportioning is 50wt.%
2-BN composite powder 55g packs in the mould of φ 190 * φ 50 * 150mm, through 30MPa pressure precompressed 20min, composite powder is in the mould mid-way, to pack in the electric current sintering system (electric current sintering equipment+radiant heating device) that is with radiant heating device through the mould of precompressed, vacuumize after fire door is airtight, at vacuum tightness 15Pa with interior sintered sample, 300 ℃/min of temperature rise rate, 1800 ℃ of sintering temperatures, sintering pressure 30MPa, insulation 3min, insulation finishes the power supply that the back cuts off current flow heats and radiation heating, naturally cooling obtains the closely knit block materials of even structure.Current flow heats power supply and radiation heating power supply are worked simultaneously, and matching way adopts mold surface temperature consistent with radiation heating heating element temperature.
Embodiment 2:
A kind of current flow heats is in conjunction with the dual heating mode flash sintering method of radiation heating, and 1, at first in electric current sintering equipment, disposed radiant heating device (as Fig. 1, Fig. 2, Fig. 3, shown in Figure 4) than 20: 1 by current flow heats power and radiation heating power; Radiation heating heating element 3 installation sites of radiant heating device are between the chamber wall 4 of mould 2 outsides and electric current sintering equipment, 4 floor height temperature thermofins are set between the chamber wall of described radiation heating heating element and electric current sintering equipment, and high temperature insulating layer material is carbon fiber felt; Radiation heating heating element height and mold height were with 1: 1 coupling, and the radiation heating heating element is a round shape, and radiant heating device has and overlaps independently power supply and supply with and temperature measuring system.
2, the flash sintering method of current flow heats and radiation heating dual heating mode prepares Al
2O
3Thin brilliant pottery (sample 1) is with the Al of median size 600nm
2O
3Powder 3g packs in the mould of φ 40 * φ 15 * 50mm, through 30MPa pressure precompressed 20min, Al
2O
3Powder is in the mould mid-way, to pack in the electric current sintering system (electric current sintering equipment+radiant heating device) that is with radiant heating device through the mould of precompressed, vacuumize after fire door is airtight, at vacuum tightness 15Pa with interior sintered sample, 800 ℃/min of temperature rise rate, 1650 ℃ of sintering temperatures, sintering pressure 50MPa, be not incubated, cut off the power supply of current flow heats and radiation heating, naturally cooling obtains the closely knit block grained material of even structure.Current flow heats power supply and radiation heating power supply are worked simultaneously, and matching way adopts mold surface temperature consistent with radiation heating heating element temperature.
Analyze through scanning electronic microscope (SEM) (referring to Fig. 5) and transmission electron microscope (TEM) (referring to Fig. 6), material internal even structure, closely knit, and crystal grain is tiny, and when selecting the raw material powder of 600nm for use, the inner crystal grain of closely knit block materials is less than 1 μ m.Adopt the flash sintering method of current flow heats and radiation heating dual heating mode to prepare the uniform closely knit block materials of structure.
Embodiment 3:
A kind of current flow heats is in conjunction with the dual heating mode flash sintering method of radiation heating, and 1, at first in electric current sintering equipment, disposed radiant heating device (as shown in Figure 1 and Figure 2) than 30: 1 by current flow heats power and radiation heating power; Radiation heating heating element 3 installation sites of radiant heating device are between the chamber wall 4 of mould 2 outsides and electric current sintering equipment, 1 floor height temperature thermofin is set between the chamber wall of described radiation heating heating element and electric current sintering equipment, and high temperature insulating layer material is carbon fiber felt; Radiation heating heating element height and mold height be with 3: 2 couplings, and the radiation heating heating element is for disperse installing shape, and radiant heating device has and overlaps independently power supply and supply with and temperature measuring system.
2, the flash sintering method of current flow heats and radiation heating dual heating mode prepares Al-Mg alloy (sample 1), the Al-Mg alloy powder 10g of median size 25 μ m is packed in the mould of φ 90 * φ 30 * 80mm, the Al-Mg alloy powder is in the mould mid-way, vacuumize, at vacuum tightness 15Pa with interior sintered sample, 500 ℃/min of temperature rise rate, 500 ℃ of sintering temperatures, sintering pressure 30MPa, insulation 3min, insulation finishes the power supply that the back cuts off current flow heats and radiation heating, naturally cooling obtains the closely knit block materials of even structure.Current flow heats power supply and radiation heating power supply are worked simultaneously, and matching way adopts mold surface temperature consistent with radiation heating heating element temperature.
The above, it only is preferred embodiment of the present invention, be not that the present invention is done any pro forma restriction, every foundation technical spirit of the present invention all still belongs in the scope of technical solution of the present invention any simple modification, equivalent variations and modification that above embodiment did.
Claims (5)
1. a current flow heats is in conjunction with the dual heating mode flash sintering method of radiation heating, it is characterized in that in electric current sintering equipment, disposing radiant heating device than 30: 1～5: 1 by current flow heats power and radiation heating power, the radiation heating heating element installation site of radiant heating device is between the chamber wall of the mould outside and electric current sintering equipment, and radiation heating heating element height and mold height were with 1: 2～3: 2 couplings; At the sintering diameter during greater than the sample of 30mm, adopt Fast Sintering under current flow heats and the radiation heating dual heating mode, mold surface temperature and radiation heating heating element temperature gap be controlled at mold surface temperature 15% in, temperature rise rate is controlled at 100～800 ℃/min in the temperature-rise period, and soaking time is controlled at 3～15min; When the sintering diameter is less than or equal to the sample of 30mm, adopt Fast Sintering under current flow heats and the radiation heating dual heating mode, mold surface temperature and radiation heating heating element temperature gap be controlled at mold surface temperature 15% in, temperature rise rate is controlled at 800～1000 ℃/min in the temperature-rise period, and soaking time is controlled at 0～3min; Insulation finishes the power supply that the back cuts off current flow heats and radiation heating, naturally cooling.
2. a kind of current flow heats according to claim 1 is characterized in that in conjunction with the dual heating mode flash sintering method of radiation heating: described radiant heating device has and overlaps independently power supply and supply with and temperature measuring system.
3. a kind of current flow heats according to claim 1 is characterized in that in conjunction with the dual heating mode flash sintering method of radiation heating: described radiation heating heating element is round shape, square tube shape or disperses shape is installed that radiation heating heating element material is a graphite.
4. a kind of current flow heats according to claim 1 is in conjunction with the dual heating mode flash sintering method of radiation heating, it is characterized in that: 1-10 floor height temperature thermofin is set between the chamber wall of described radiation heating heating element and electric current sintering equipment, and high temperature insulating layer material is carbon fiber felt.
5. a kind of current flow heats according to claim 1 is characterized in that in conjunction with the dual heating mode flash sintering method of radiation heating: described sample is stupalith, ceramic matric composite, metal or metal-base composites.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2007100517766A CN100516000C (en) | 2007-03-30 | 2007-03-30 | Dual heating mode flash sintering method combining current heating with radiant heating |
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| CNB2007100517766A CN100516000C (en) | 2007-03-30 | 2007-03-30 | Dual heating mode flash sintering method combining current heating with radiant heating |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109734445A (en) * | 2019-03-06 | 2019-05-10 | 武汉理工大学 | A kind of electric field-assisted flash sintering method of Ultra-fine Grained hafnium oxide ceramics |
| CN109761619A (en) * | 2019-03-11 | 2019-05-17 | 武汉理工大学 | A kind of boron nitride ceramics and preparation method thereof and Preparation equipment |
| CN109761620A (en) * | 2019-03-05 | 2019-05-17 | 武汉理工大学 | A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride |
| CN112153764A (en) * | 2020-09-28 | 2020-12-29 | 中国农业大学 | Rapid heating method for preparing ceramic material |
-
2007
- 2007-03-30 CN CNB2007100517766A patent/CN100516000C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761620A (en) * | 2019-03-05 | 2019-05-17 | 武汉理工大学 | A kind of method that dual heating mode discharge plasma sintering prepares compact silicon nitride |
| CN109734445A (en) * | 2019-03-06 | 2019-05-10 | 武汉理工大学 | A kind of electric field-assisted flash sintering method of Ultra-fine Grained hafnium oxide ceramics |
| CN109761619A (en) * | 2019-03-11 | 2019-05-17 | 武汉理工大学 | A kind of boron nitride ceramics and preparation method thereof and Preparation equipment |
| CN112153764A (en) * | 2020-09-28 | 2020-12-29 | 中国农业大学 | Rapid heating method for preparing ceramic material |
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| CN100516000C (en) | 2009-07-22 |
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Granted publication date: 20090722 Termination date: 20140330 |