CN106630974A - Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof - Google Patents
Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof Download PDFInfo
- Publication number
- CN106630974A CN106630974A CN201611061915.9A CN201611061915A CN106630974A CN 106630974 A CN106630974 A CN 106630974A CN 201611061915 A CN201611061915 A CN 201611061915A CN 106630974 A CN106630974 A CN 106630974A
- Authority
- CN
- China
- Prior art keywords
- ceramic
- sintering
- ceramics
- flash
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/583—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on boron nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
-
- 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
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/02—Furnaces of a kind not covered by any preceding group specially designed for laboratory use
-
- 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
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/08—Heating by electric discharge, e.g. arc discharge
- F27D11/10—Disposition of electrodes
Abstract
The invention relates to the filed of ceramic sintering, in particular to a flash sintering method of a low-temperature flash sintering ceramic and an obtained ceramic and a device thereof. The flash sintering method of the low-temperature flash sintering ceramic comprises the following steps: loading a voltage at two ends of a ceramic green body, and setting a current upper limit; heating the ceramic green body, when the temperature reaches a characteristic temperature, the temperature suddenly rising and meanwhile bright spots appearing around an anode, then a flash phenomenon appearing, and completing sintering of the ceramic green body within several seconds. According to the method, the flash phenomenon occurs when the temperature is heated to a certain characteristic temperature through voltage assist, and the sintering is completed within several seconds, so that the sintering temperature can be effectively reduced, and the sintering time can be greatly shortened. Moreover, according to the sintering method, the energy resources are saved, the sintering efficiency is improved, the production cost is reduced, ceramic products with large dimensions and complicated shapes can be produced, the density of a sintered ceramic block body is generally more than 95%, and the quality of the sintered and obtained ceramic is excellent.
Description
Technical field
The present invention relates to ceramic post sintering field, in particular to a kind of flash of light sintering side of low temperature Fast Sintering ceramics
Method and obtained ceramics and its device.
Background technology
Fast Sintering is the main trend of ceramic sintering technology in the world in recent years.Meet the burning of Fast Sintering requirement at present
Knot technology is mainly discharge plasma sintering (SPS).Plasma be dissociation high-temperature electric conduction gas, the higher shape of reactivity
State.Because plasma temperature is typically at 4000～10999 DEG C, its gaseous molecular and atom are in advanced activation state, and wait
Degree of ionization is very high in ionized gas, and these properties cause plasma to become a kind of very important material preparation and process
Technology.The sintering process is caused particle equably itself to produce Joule heat and is made particle surface activation become electric discharge using pulse current
Plasma, accelerates diffusion process so that bridge joint and then at a lower temperature Fast Sintering are easier to make between ceramic particle
Powder is fine and close.SPS technologies have the advantages that quickly, low temperature, high efficiency, can be used to prepare metal, ceramics, nano material, amorphous
Material, composite, functionally gradient material (FGM) etc., therefore a large amount of concerns and research of educational circles and industry have been obtained in recent years.Wherein study
Most is functional material, including thermoelectric material, magnetic material, FGM, composite functional material and nano functional material
Material etc..Additionally, prepare SPS in non-crystaline amorphous metal, marmem, diamond etc. also to have made to attempt.At present abroad, especially
Japan has carried out the research that more multiplex SPS prepares new material, and portioned product puts into production.
However, the sintering basis mechanism of SPS is not fully understood at present, needs carry out a large amount of practices have been come with theoretical research
It is kind.Current SPS there is no method sintering to accomplish complete densification more than the product of 300mm sizes due to the capacity limit of pulse current.
And, SPS current design there is no method to make complex-shaped product.In addition, the price of SPS is costly, although there is industry
The product of change, but sinter relatively costly, the still less production for being applied to actual ceramic product at present.
In view of this, it is special to propose the present invention.
The content of the invention
The first object of the present invention is to provide a kind of flash of light sintering method of low temperature Fast Sintering ceramics, and the method passes through
Voltage is aided in, and when temperature is heated to certain characteristic temperature, phosphere occurs, and completes to sinter within the several seconds, and this feature temperature
200 DEG C lower than the common pressureless sintering temperature of respective material and more than, so not only can effectively reduce sintering temperature, but also can
Greatly shorten sintering time.Additionally, the sintering process energy saving, raising sinter efficiency, reduce production cost and can produce big chi
Very little complex-shaped ceramic product, the ceramic block density of sintering is typically more than 95%, and the ceramic mass that sintering is obtained
It is superior.
The second object of the present invention is the dress of the flash of light sintering method for providing the low temperature Fast Sintering ceramics for implementing described
Put.
In order to realize the above-mentioned purpose of the present invention, spy employs the following technical solutions：
A kind of flash of light sintering method of low temperature Fast Sintering ceramics, comprises the following steps：
In ceramic green two ends on-load voltage, the setting electric current upper limit；
The ceramic green is heated, after phosphere occurs in surrounding them, deenergization, insulation, cooling completes to burn
Knot.
Wherein, the electric current of setting is arranged according to following methods：First to ceramic green under certain voltage such as 200-
Preliminary experiment is carried out under 1000V/cm voltages, when being heated to characteristic temperature, electric current rises sharply while there is the phosphere of electrical breakdown, and
The upper current limit of setting is the electric current that electrical breakdown does not occur, that is, the upper current limit for arranging is less than electric current during electrical breakdown.Therefore, root
Corresponding upper current limit is selected according to preliminary experiment.
A kind of flash of light sintering method of low temperature Fast Sintering ceramics that the present invention is provided, the sintering process is existed using certain ceramics
The principle that resistance is gradually lowered in temperature-rise period, when temperature is increased to some critical point, i.e. temperature certain characteristic temperature is heated to
When, is there is shining point by the resistance of ceramic green to a relatively low resistance level and simultaneously in positive pole in rapid drawdown.It is fixed according to ohm
Rule, now will have great electric current moment by ceramic green on ceramic green, therefore the very short time after shining point occurs
The interior phenomenon for producing similar electrical breakdown, in the short period of time Fast Sintering is fine and close to make ceramic green.Green compact after sintering due to
Resistance is raised, and lightning phenomenon disappears therewith, until sintering is completed.The process of flash of light sintering is tied from there is shining point to phosphere
Beam, completes sintering within the several seconds.The present invention aids in the characteristic temperature that reaches than the common pressureless sintering of respective material by voltage
Temperature it is low 200 DEG C and more than, so not only can effectively reduce sintering temperature, but also be substantially shorter sintering time.The sintering
Method energy saving, the ceramic product for improving sintering efficiency, reducing production cost and oversized shape complexity can be produced, the pottery of sintering
Porcelain block density is typically more than 95%.
Inventor has found that the consistency of obtained ceramic green is higher, then the sintering temperature for needing in temperature-rise period is lower,
And the ceramic performance that sintering is obtained is more preferably.
Further, the ceramic powders particle mean size used by the ceramic green is less than 500nm.
Preferably, the density of the ceramic green 50% and more than.
The drawing method of green compact includes colding pressing, isostatic cool pressing and moulding by casting etc..
Find in process of the test, ceramic green thickness is thinner, sinter the ceramic performance for obtaining more preferably.Preferably, it is described
The thickness of ceramic green is 2mm-2cm.Such as the thickness of ceramic green can be 2mm, 5mm, 1cm, 2cm.
Further, the corresponding power supply of on-load voltage is direct current or the one kind in AC power, and the scope of voltage is not
More than 2000V/cm.Such as can be 100V/cm, 500V/cm, 1000V/cm, 1500V/cm, 2000V/cm.The voltage model
In enclosing, according to the concrete material for selecting, the current limit upper limit, phosphere can occur in its characteristic temperature, effectively reduce
Sintering temperature.
Further, the mode in ceramic green two ends on-load voltage be green compact two ends drilling loading electrode or
Using high-temperature electric conduction glue by electrode and green compact adhesion；
Electrode used is metal electrode or graphite electrode.
Further, in the ceramic green sintering process, do not carry extra pressure, sintering atmosphere be air, vacuum and
Any one in non-air gas.
During sintering, the ceramics used by ceramic green are oxide ceramic, and the atmosphere of sintering selects air；If used by ceramic green
Ceramics be non-oxidation ceramic, the atmosphere of sintering is typically from vacuum or non-air gas.
Further, the time of the insulation is within 10 minutes；Then dropped with the speed for being not more than 5 DEG C/min
Temperature.To obtain the good ceramic product of crystal formation, and prevent the crackle caused because cooling rate is too fast.
Further, the ceramics used by the ceramic green are oxide ceramic or non-oxidation ceramic；
The oxide ceramic includes aluminum oxide, zirconia ceramics and its compound etc.；
The non-oxidation ceramic includes nitride ceramics, carbide ceramics and cermet and its compound etc.；
The nitride ceramics includes silicon nitride ceramics, boron nitride ceramics and its compound etc.；
The carbide ceramics includes silicon carbide ceramics and its compound etc..
Present invention also offers ceramics obtained in the flash of light sintering method of above-mentioned low temperature Fast Sintering ceramics.
Present invention also offers implement the device of the flash of light sintering method of above-mentioned low temperature Fast Sintering ceramics, including tubular type
Electrode is loaded in stove, the tube furnace, and the electrode stretches out from the tube furnace and is connected with outside power supply；
The tube furnace is additionally provided with the position of observation window, the loading electrode and the observation window and is provided with cooling dress
Put.
What the present invention was provided implements the device of the flash of light sintering method of above-mentioned low temperature Fast Sintering ceramics, and simple structure is
The sintering of ceramics is provided very big facility.
Wherein, in the device that the present invention is provided, observation window can be being connected with image data acquiring and processing system.
Further, the observation window is arranged at the flange of the inlet end of the tube furnace, and the electrode is by described
The flange of the outlet side of tube furnace stretches out.
Device in the present invention can be converted by high temperature process furnances, specifically, including tube furnace, device for cooling flange,
Electrode, power supply, observation window and the image data acquiring being connected with observation window and processing system.Tube furnace is in sealing ventilation atmosphere
Pattern under can prepare non-oxide ceramicses, oxide ceramics can be prepared under unsealed pattern.The air inlet hold-carrying of tube furnace
Blue place has installed observation window additional, the image viewing being available in testing；The flange of outlet side has installed platinum electrode additional for sintered
The voltage-drop loading of the green compact in journey, the electrode high-temperature resistant rubber guarantees insulation with flange.Because tube furnace is high temperature process furnances,
And the requests for alternations of observation window and electrode does not use boiler tube plug on flange, flange can be caused at high temperature to cross heat affecting picture number
According to collection and the loading of electric charge, accordingly, it would be desirable to cooling device, i.e., carry out the loading and repacking of water cooling plant to flange, and make
Use recirculated water cold.Meanwhile, device for cooling flange can extend the service life of closed rubber ring, and improve boiler tube in ventilation atmosphere
Pattern under air-tightness.Loading power carries out electric charge during heating and sintering by two platinum wires to ceramic green
Loading, with realize green compact flash of light sinter.The power supply is orthogonal stream integrated power supply, can be entered under direct current or the pattern of exchange
Row flash of light sintering, peak power is 3000-4000 watt.The power supply possesses the real time data output function of voltage source.Additionally, also
Image data acquiring and processing system can be equipped with, the process of flash of light sintering furnace is recorded by observation window, and real time record adds
(power supply need to possess the function of voltage x current data output in real time to the voltage and current signal of load power supply, and computer need to be equipped with electricity
The Real-time Collection software of piezoelectricity flow data), be available for study in Germicidal efficacy and data record.
Compared with prior art, beneficial effects of the present invention are：
(1) a kind of flash of light sintering method of low temperature Fast Sintering ceramics that the present invention is provided, is aided in, in temperature by voltage
When being heated to certain characteristic temperature, there is phosphere, sintering is completed within the several seconds, and this feature temperature is more common than respective material
Pressureless sintering temperature it is low 200 DEG C and more than, so not only can effectively reduce sintering temperature, but also when being substantially shorter sintering
Between.
(2) the sintering process energy saving of present invention offer, raising sinters efficiency, reduces production cost and can produce large scale
Complex-shaped ceramic product, the ceramic block density of sintering is typically more than 95%, and the ceramic mass that sintering is obtained is excellent
More.
(3) present invention also offers implementing the device of the flash of light sintering method of low temperature Fast Sintering ceramics, simple structure is
The sintering of ceramics carries out offer facility.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described.
Fig. 1 is the schematic diagram of the flash of light sintering furnace that the embodiment of the present invention 1 is provided；
Fig. 2 is the profile of the flash of light sintering furnace that the embodiment of the present invention 1 is provided；
In figure：1- tube furnaces；2- device for cooling flange；3- electrodes；4- power supplys；5- observation windows.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will
Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the present invention.It is unreceipted concrete in embodiment
Condition person, the condition advised according to normal condition or manufacturer is carried out.Agents useful for same or the unreceipted production firm person of instrument, are
The conventional products that commercially available purchase is obtained can be passed through.
Embodiment 1
The present invention is provided with a set of device for implementing the flash of light sintering method of low temperature Fast Sintering ceramics, and the device is
A set of flash of light sintering furnace (MX-100).In the Equipment Foundations, the flash of light sintering of ceramics can be carried out.
MX-100 is by tube furnace 1, device for cooling flange 2, electrode 3, power supply 4, observation window 5 and the figure being connected with observation window
As data acquisition and processing system.Tube furnace 1 can prepare non-oxide ceramicses under the pattern of sealing ventilation atmosphere, in non-tight
Pattern under can prepare oxide ceramics, maximum temperature up to 1700 degrees Celsius, therefore, can meet great majority oxidation and it is non-oxide
The preparation demand of ceramics.
The inlet end flange of tube furnace 1 has installed observation window 5 additional, the image viewing being available in testing；The flange of outlet side
Place has installed platinum electrode additional for the voltage-drop loading of the ceramic green in sintering process, and the electrode high-temperature resistant rubber is true with flange
Protect insulation.
Because the requests for alternations that tube furnace is observation window 5 and electrode 3 on high temperature process furnances, and flange does not use boiler tube
Plug, can cause at high temperature flange to cross the loading of heat affecting image data acquiring and electric charge, it is therefore desirable to cooling device, i.e., to method
Orchid carries out the loading and repacking of water cooling plant, and using recirculated water cold.Meanwhile, device for cooling flange can extend closed rubber
The service life of circle, and improve air-tightness of the boiler tube under the pattern of ventilation atmosphere.
Loading power carries out the loading of electric charge by two platinum wires during heating and sintering to ceramic green, with
Realize the flash of light sintering of green compact.The power supply is orthogonal stream integrated power supply, can carry out flash of light burning under direct current or the pattern of exchange
Knot, peak power is 3000-4000 watt.The power supply possesses the real time data output function of voltage source.MX-100 is equipped with figure
As data acquisition and processing system, the process of the sintering furnace that glistened by observation window record, and real time record loading power
(power supply need to possess the function of voltage x current data output in real time to voltage and current signal, and computer need to be equipped with voltage x current number
According to Real-time Collection software), be available for study in Germicidal efficacy and data record.
Embodiment 2
Ceramic green is sintered using the device in embodiment 1, is comprised the following steps that：
The ceramic green of oxygenerating zircon ceramic nano powder, zirconium oxide are pushed in the pressure of 200MPa first with isostatic cool pressing
Ceramic powder purity is 99.95%, and average grain diameter is 160nm, and the ceramic green density after isostatic cool pressing is 60%, and thickness is 1cm；
Drill at the two ends of green compact, inserted in the hole the green compact that are fastened with platinum electrode, interelectrode distance is about 100mm；
Electrode is run wires on dc source, to turn on the power, power supply 200V/cm, the setting electric current upper limit is given
0.5A；
Setting tube furnace heating program：From the beginning of room temperature, 1000 degrees Celsius are heated up to 8 degrees Celsius per minute of speed,
Then 1400 degrees Celsius are warming up to 5 degrees Celsius per minute of speed；
Later on heating program, opens water cooling unit, starts simultaneously at the collection of image data acquiring and voltage x current data；
When furnace temperature rises to 1280-1350 degree Celsius of interval, can see that little Bai occurs in positive pole by image capturing system
Point, subsequently hot spot expands within the several seconds, the phosphere for similar electrical breakdown then occur, and at the same time, voltage x current data are adopted
Collecting system shows that electric current is rapidly increased to the upper limit of 0.5A, and afterwards voltage begins to decline after electric current rises to higher limit；
After phosphere terminates, immediately disconnect ceramic block on load power supply, while insulation 5 minutes, subsequently with per point
The speed that 5 degrees Celsius of clock starts cooling；
After furnace temperature is down to room temperature, water cooling unit is closed, unload electrode, take out ceramic block.
Obtained zirconia ceramics block Jing determines its density for 5.75g/cm3。
Embodiment 3
Ceramic green is sintered using the device in embodiment 1, is comprised the following steps that：
The ceramic green of preparing silicon carbide ceramic nano powder, carborundum are pushed in the pressure of 200MPa first with isostatic cool pressing
Ceramic powder purity is 99.5%, and average grain diameter is 80nm, and the ceramic green density after isostatic cool pressing is 55%, and thickness is 2mm；
Drill at the two ends of ceramic green, inserted in the hole the green compact that are fastened with platinum electrode, interelectrode distance is about
100mm；
Electrode is run wires on dc source, to turn on the power, power supply 1000V/cm, the setting electric current upper limit is given
0.5A；
Setting tube furnace heating program：From the beginning of room temperature, 1000 degrees Celsius are heated up to 8 degrees Celsius per minute of speed,
Then 1650 degrees Celsius are warming up to 5 degrees Celsius per minute of speed；
Lead to argon gas atmosphere in tube furnace boiler tube, flow velocity is 200ml/min；
Later on heating program, opens water cooling unit, starts simultaneously at the collection of image data acquiring and voltage x current data；
When furnace temperature rises to 1600-1650 degree Celsius of interval, can see that little Bai occurs in positive pole by image capturing system
Point, subsequently hot spot expands within the several seconds, the phosphere for similar electrical breakdown then occur, and at the same time, voltage x current data are adopted
Collecting system shows that electric current is rapidly increased to the upper limit of 0.5A, and afterwards voltage begins to decline after electric current rises to higher limit；
After phosphere terminates, immediately disconnect ceramic block on load power supply, while insulation 5 minutes, subsequently with per point
The speed that 5 degrees Celsius of clock starts cooling；
After furnace temperature is down to room temperature, water cooling unit is closed, unload electrode, take out ceramic block.
Obtained silicon carbide ceramics block density is 3.10g/cm3。
Embodiment 4
Ceramic green is sintered using the device in embodiment 1, is comprised the following steps that：
The ceramic green of preparing silicon carbide ceramic nano powder, carborundum are pushed in the pressure of 200MPa first with isostatic cool pressing
Ceramic powder purity is 99.5%, and average grain diameter is 450nm, and the ceramic green density after isostatic cool pressing is 50%, and thickness is 2cm；
Drill at the two ends of ceramic green, inserted in the hole the green compact that are fastened with platinum electrode, interelectrode distance is about
100mm；
Electrode is run wires on dc source, to turn on the power, power supply 2000V/cm, the setting electric current upper limit is given
0.4A；
Setting tube furnace heating program：From the beginning of room temperature, 1000 degrees Celsius are heated up to 8 degrees Celsius per minute of speed,
Then 1650 degrees Celsius are warming up to 5 degrees Celsius per minute of speed；
Lead to argon gas atmosphere in tube furnace boiler tube, flow velocity is 200ml/min；
Later on heating program, opens water cooling unit, starts simultaneously at the collection of image data acquiring and voltage x current data；
When furnace temperature rises to 1600-1650 degree Celsius of interval, can see that little Bai occurs in positive pole by image capturing system
Point, subsequently hot spot expands within the several seconds, the phosphere for similar electrical breakdown then occur, and at the same time, voltage x current data are adopted
Collecting system shows that electric current is rapidly increased to the upper limit of 0.4A, and afterwards voltage begins to decline after electric current rises to higher limit；
After phosphere terminates, immediately disconnect ceramic block on load power supply, while insulation 5 minutes, subsequently with per point
The speed that 3 degrees Celsius of clock starts cooling；
After furnace temperature is down to room temperature, water cooling unit is closed, unload electrode, take out ceramic block.
Obtained silicon carbide ceramics block density is 3.05g/cm3。
Embodiment 5
Ceramic green is sintered using the device in embodiment 1, is comprised the following steps that：
The ceramic green of boron nitride ceramics nano powder, boron nitride are suppressed under the pressure of 200MPa first with isostatic cool pressing
Ceramic powder purity is 99%, and average grain diameter is 150nm, and the ceramic green density after isostatic cool pressing is 60%, and thickness is 5mm；
Drill at the two ends of ceramic green, inserted in the hole the green compact that are fastened with platinum electrode, interelectrode distance is about
80mm；
Electrode is run wires on dc source, to turn on the power, power supply 2000V/cm, the setting electric current upper limit is given
0.5A；
Setting tube furnace heating program：From the beginning of room temperature, 1000 degrees Celsius are heated up to 8 degrees Celsius per minute of speed,
Then 1600 degrees Celsius are warming up to 5 degrees Celsius per minute of speed；
Lead to nitrogen atmosphere in tube furnace boiler tube, flow velocity is 200ml/min；
Later on heating program, opens water cooling unit, starts simultaneously at the collection of image data acquiring and voltage x current data；
When furnace temperature rises to 1500-1600 degree Celsius of interval, can see that little Bai occurs in positive pole by image capturing system
Point, subsequently hot spot expands within the several seconds, the phosphere for similar electrical breakdown then occur, and at the same time, voltage x current data are adopted
Collecting system shows that electric current is rapidly increased to the upper limit of 0.5A, and afterwards voltage begins to decline after electric current rises to higher limit；
After phosphere terminates, immediately disconnect ceramic block on load power supply, while insulation 5 minutes, subsequently with per point
The speed that 4 degrees Celsius of clock starts cooling；
After furnace temperature is down to room temperature, water cooling unit is closed, unload electrode, take out ceramic block.
Obtained boron nitride ceramics block density is 2.16g/cm3。
Although illustrate and describing the present invention with specific embodiment, but will be appreciated that without departing substantially from the present invention's
Many other changes and modification can be made in the case of spirit and scope.It is, therefore, intended that in the following claims
Including all such changes and modifications belonged in the scope of the invention.
Claims (10)
1. the flash of light sintering method of a kind of low temperature Fast Sintering ceramics, it is characterised in that comprise the following steps：
In ceramic green two ends on-load voltage, the setting electric current upper limit；
The ceramic green is heated, after phosphere occurs in surrounding them, deenergization, insulation, cooling completes sintering.
2. the flash of light sintering method of low temperature Fast Sintering according to claim 1 ceramics, it is characterised in that the ceramic green
Ceramic powders particle mean size used by base is less than 500nm；
Preferably, the density of the ceramic green 50% and more than；
Preferably, the thickness of the ceramic green is 2mm-2cm.
3. the flash of light sintering method of low temperature Fast Sintering according to claim 1 ceramics, it is characterised in that on-load voltage pair
The power supply answered is direct current or the one kind in AC power, and the scope of voltage is not more than 2000V/cm.
4. the flash of light sintering method of low temperature Fast Sintering according to claim 3 ceramics, it is characterised in that in the ceramics
The mode of green compact two ends on-load voltage is by electrode and green compact in green compact two ends drilling loading electrode or using high-temperature electric conduction glue
Adhesion；
Electrode used is metal electrode or graphite electrode.
5. the flash of light sintering method of low temperature Fast Sintering according to claim 1 ceramics, it is characterised in that the ceramic green
In base sintering process, extra pressure is not carried, sintering atmosphere is any one in air, vacuum and non-air gas.
6. the ceramic flash of light sintering method of low temperature Fast Sintering according to any one of claim 1-5, it is characterised in that institute
The time of insulation is stated within 10 minutes；Then lowered the temperature with the speed for being not more than 5 DEG C/min.
7. the ceramic flash of light sintering method of low temperature Fast Sintering according to any one of claim 1-5, it is characterised in that institute
It is oxide ceramic or non-oxidation ceramic to state the ceramics used by ceramic green；
The oxide ceramic includes aluminum oxide, zirconia ceramics and its compound etc.；
The non-oxidation ceramic includes nitride ceramics, carbide ceramics and cermet and its compound etc.；
The nitride ceramics includes silicon nitride ceramics, boron nitride ceramics and its compound etc.；
The carbide ceramics includes silicon carbide ceramics and its compound etc..
8. ceramic obtained in the flash of light sintering method of the low temperature Fast Sintering ceramics described in any one of claim 1-7.
9. the device of the ceramic sintering method that glistens of the low temperature Fast Sintering described in any one of claim 1-7, its feature are implemented
It is, including tube furnace, loading electrode in the tube furnace, and the electrode stretch out and outside electricity from the tube furnace
Source connects；
The tube furnace is additionally provided with the position of observation window, the loading electrode and the observation window and is provided with cooling device.
10. device according to claim 9, it is characterised in that the observation window is arranged at the inlet end of the tube furnace
Flange, the electrode stretched out by the flange of the outlet side of the tube furnace.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611061915.9A CN106630974A (en) | 2016-11-25 | 2016-11-25 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611061915.9A CN106630974A (en) | 2016-11-25 | 2016-11-25 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106630974A true CN106630974A (en) | 2017-05-10 |
Family
ID=58811802
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611061915.9A Pending CN106630974A (en) | 2016-11-25 | 2016-11-25 | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106630974A (en) |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107202495A (en) * | 2017-06-26 | 2017-09-26 | 中国工程物理研究院材料研究所 | Flash burning structure and flash burning stove |
| CN107881560A (en) * | 2017-11-24 | 2018-04-06 | 苏州阿特斯阳光电力科技有限公司 | A kind of preprocess method of crystalline silicon rod |
| CN108821767A (en) * | 2018-06-20 | 2018-11-16 | 苏州山人纳米科技有限公司 | A kind of preparation method of compound zirconia pottery backboard |
| CN108911752A (en) * | 2018-08-01 | 2018-11-30 | 渤海大学 | A method of synthesizing ceramic material under the conditions of extra electric field |
| CN108947531A (en) * | 2018-08-21 | 2018-12-07 | 苏州山人纳米科技有限公司 | The flash burning preparation method of rare earth oxide transparent ceramic scintillator |
| CN109534809A (en) * | 2019-01-22 | 2019-03-29 | 陕西科技大学 | A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted |
| CN109678498A (en) * | 2019-01-22 | 2019-04-26 | 陕西科技大学 | A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics |
| CN110357633A (en) * | 2019-07-11 | 2019-10-22 | 上海交通大学 | A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic |
| CN110590373A (en) * | 2019-10-28 | 2019-12-20 | 中原工学院 | MoSi prepared by Flashing method2Method for preparing-MoB-SiC three-phase composite material |
| CN110590374A (en) * | 2019-10-28 | 2019-12-20 | 中原工学院 | MoSi prepared by Flashing method2Method for producing-SiC composite material |
| CN111362707A (en) * | 2020-04-03 | 2020-07-03 | 清华大学深圳国际研究生院 | Room temperature ceramic sintering method and ceramic |
| CN111440002A (en) * | 2020-04-03 | 2020-07-24 | 清华大学深圳国际研究生院 | Ceramic sintering method and ceramic sintering device |
| CN113149619A (en) * | 2021-05-14 | 2021-07-23 | 景德镇陶瓷大学 | High-strength low-dielectric-loss alumina ceramic substrate |
| CN114199032A (en) * | 2021-12-21 | 2022-03-18 | 清华大学深圳国际研究生院 | Plasma-assisted ceramic sintering device and ceramic sintering method |
| CN115894058A (en) * | 2022-11-25 | 2023-04-04 | 南京航空航天大学 | Method for flash-burning rapid densification of SiC/SiC composite material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140548A (en) * | 2015-07-01 | 2015-12-09 | 北京理工大学 | Sintering method of electrolytes for solid oxide fuel cell |
| CN106116559A (en) * | 2016-08-30 | 2016-11-16 | 西南交通大学 | A kind of electric field-assisted ceramic low-temp quick-combustion device |
-
2016
- 2016-11-25 CN CN201611061915.9A patent/CN106630974A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140548A (en) * | 2015-07-01 | 2015-12-09 | 北京理工大学 | Sintering method of electrolytes for solid oxide fuel cell |
| CN106116559A (en) * | 2016-08-30 | 2016-11-16 | 西南交通大学 | A kind of electric field-assisted ceramic low-temp quick-combustion device |
Non-Patent Citations (1)
| Title |
|---|
| JOHN A. DOWNS等: "Electric Field Assisted Sintering of Cubic Zirconia at 390℃", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 * |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107202495A (en) * | 2017-06-26 | 2017-09-26 | 中国工程物理研究院材料研究所 | Flash burning structure and flash burning stove |
| CN107881560A (en) * | 2017-11-24 | 2018-04-06 | 苏州阿特斯阳光电力科技有限公司 | A kind of preprocess method of crystalline silicon rod |
| CN108821767A (en) * | 2018-06-20 | 2018-11-16 | 苏州山人纳米科技有限公司 | A kind of preparation method of compound zirconia pottery backboard |
| CN108911752A (en) * | 2018-08-01 | 2018-11-30 | 渤海大学 | A method of synthesizing ceramic material under the conditions of extra electric field |
| CN108947531B (en) * | 2018-08-21 | 2021-05-14 | 山东晶盾新材料科技有限公司 | Flash firing preparation method of rare earth oxide transparent ceramic scintillator |
| CN108947531A (en) * | 2018-08-21 | 2018-12-07 | 苏州山人纳米科技有限公司 | The flash burning preparation method of rare earth oxide transparent ceramic scintillator |
| CN109534809A (en) * | 2019-01-22 | 2019-03-29 | 陕西科技大学 | A kind of method of the low temperature Fast Sintering barium titanate PTC ceramics of electric field-assisted |
| CN109678498A (en) * | 2019-01-22 | 2019-04-26 | 陕西科技大学 | A kind of method of low temperature Fast Sintering NBT piezoelectric ceramics |
| CN110357633A (en) * | 2019-07-11 | 2019-10-22 | 上海交通大学 | A kind of method that room temperature quickly prepares titanium aluminium-carbon ceramic |
| CN110590373A (en) * | 2019-10-28 | 2019-12-20 | 中原工学院 | MoSi prepared by Flashing method2Method for preparing-MoB-SiC three-phase composite material |
| CN110590374A (en) * | 2019-10-28 | 2019-12-20 | 中原工学院 | MoSi prepared by Flashing method2Method for producing-SiC composite material |
| CN111440002A (en) * | 2020-04-03 | 2020-07-24 | 清华大学深圳国际研究生院 | Ceramic sintering method and ceramic sintering device |
| CN111362707A (en) * | 2020-04-03 | 2020-07-03 | 清华大学深圳国际研究生院 | Room temperature ceramic sintering method and ceramic |
| CN113149619A (en) * | 2021-05-14 | 2021-07-23 | 景德镇陶瓷大学 | High-strength low-dielectric-loss alumina ceramic substrate |
| CN114199032A (en) * | 2021-12-21 | 2022-03-18 | 清华大学深圳国际研究生院 | Plasma-assisted ceramic sintering device and ceramic sintering method |
| WO2023116162A1 (en) * | 2021-12-21 | 2023-06-29 | 清华大学深圳国际研究生院 | Plasma-assisted ceramic sintering device and ceramic sintering method |
| CN114199032B (en) * | 2021-12-21 | 2023-11-28 | 清华大学深圳国际研究生院 | Plasma-assisted ceramic sintering device and ceramic sintering method |
| CN115894058A (en) * | 2022-11-25 | 2023-04-04 | 南京航空航天大学 | Method for flash-burning rapid densification of SiC/SiC composite material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106630974A (en) | Flash sintering method of low-temperature flash sintering ceramic and obtained ceramic and device thereof | |
| Zapata-Solvas et al. | Preliminary investigation of flash sintering of SiC | |
| CN102260802B (en) | Target preparation device and target processing method thereof | |
| CN103639408B (en) | A kind of method preparing Intermatallic Ti-Al compound with titantium hydride Al alloy powder short route | |
| CN110577399B (en) | Multi-field coupling flash sintering system based on induction heating | |
| JPS6241281B2 (en) | ||
| CN111981847A (en) | Pressure-assisted induction heating vacuum atmosphere flash sintering device | |
| TW201041424A (en) | Ceramic heater and method for producing same | |
| CN110128115A (en) | A kind of method that flash burning prepares oxide eutectic ceramics | |
| CN104894641B (en) | It is a kind of high fine and close（LaxCa1‑x）B6Polycrystalline cathode material and preparation method thereof | |
| CN103194629B (en) | Method for preparing tungsten molybdenum copper composite material | |
| CN106238732A (en) | A kind of discharge plasma sintering system | |
| CN112830790B (en) | Hafnium-niobium-based ternary solid solution boride conductive ceramic and preparation method and application thereof | |
| CN109357528A (en) | A kind of ceramic material sintering furnace and its control method using electric field-assisted | |
| CN106116559B (en) | A kind of electric field-assisted ceramic low-temp quick-combustion device | |
| CN106045482B (en) | Rare earth oxide doped aluminium base high-performance metal bath determines the preparation method of HydroNit sensor material | |
| JP2019182689A (en) | Manufacturing method for sintered body and sintered body | |
| CN104014792A (en) | Method for adopting spark plasma for sintering high-performance copper tungsten electrical contact materials | |
| CN108534553A (en) | The device and method of block body ceramic material is quickly prepared using high-frequency induction heating | |
| CN104302021A (en) | Heating unit used for electrical heating and preparation technology of heating unit | |
| CN206089473U (en) | Supplementary ceramic low temperature of electric field burns device soon | |
| JP4824847B2 (en) | Method for producing ceramic eutectic | |
| CN102503380B (en) | Method for preparing alumina-base eutectic ceramics in laser surface atmosphere heating furnace | |
| CN105906347A (en) | Method for preparing nanocrystal aluminum nitride ceramics | |
| CN203037063U (en) | Sintering furnace for zirconium oxide dental restoration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170510 |