CN108947542A - The direct flash burning molding method for preparing of ceramic powder stock - Google Patents
The direct flash burning molding method for preparing of ceramic powder stock Download PDFInfo
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- 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
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The direct flash burning molding method for preparing of ceramic powder stock of the present invention, steps are as follows: (1) pouring raw material in mold into, vibration makes its surfacing；(2) mold is put into ceramic powder stock straight forming flash burning equipment, applies 40 ~ 50MPa pressure, ceramic powder stock is made to be in heating zone middle position；(3) auxiliary heating power supply (being herein induction heating power) is opened, be heated to 900 DEG C ~ 1000 DEG C with 100 DEG C/min ~ 110 DEG C/min speed or until phosphere occurs；(4) high voltage direct current flash burning power supply is opened, in sample two sides and passes to direct current, linearly increasing voltage about 200V/cm, until phosphere occurs；(5) control electric current is down to 1000A hereinafter, constant current；Continue 20~50s；(6) it is cooled to room temperature, obtains fine and close sintered body；(7) sintered body is polished directly, obtains required product.
Description
Technical field
The present invention relates to ceramic post sintering forming technique and its equipment technical field is used, specifically, it shows a kind of ceramics
The direct flash burning molding method for preparing of powder raw material.
Background technique
Ceramic material is a kind of important industrial materials, different ceramics have different mechanics, electricity, optics, acoustics,
The performances such as magnetics, thus there is colourful application, become the indispensable important materials of modern society.
The preparation process of ceramic material is varied, generally uses molding-sintering-mechanical processing technique process.Sintering is
A mostly important process in ceramic material preparation process, it is the important link for feeling material property.In traditional high temperature
In sintering process, it needs to consume a large amount of energy, may cause serious environmental problem.In order to it is energy saving, protection environment,
Many novel sintered technologies are developed, such as the sintering of microwave sintering, HIP sintering, discharge plasma.
These new technologies have application in different fields, are made that significant contribution for the development of ceramic material.2010
Rishi Raj proposes a kind of new ceramic post sintering method, flash burning method.Flash burning technology can realize the cause of ceramics in a few seconds
Densification, while sintering temperature is greatly reduced, thus there is the advantages of high-efficient, low energy consumption.Many researchs on this basis
Person proposes various agglomerating plant based on flash burning principle in succession.
As described a kind of electric field-assisted ceramics using panel heater metal electrode in 206089473 U of patent CN
Low temperature fast firing device is easy to observing and controlling sintering process its advantage is that can work in air atmosphere.107202495 A of CN is proposed
Using the flash burning structure of hydraulic press metal electrode, it can be used for suppressing the flash burning sintering of green compact.
But existing agglomerating plant is only used for the preparation of crude green body and green compact, can not carry out the preparation of fine and close sintered body.
Therefore, it is necessary to provide a kind of direct flash burning molding method for preparing of ceramic powder stock to solve the above problems.
Summary of the invention
The object of the present invention is to provide a kind of direct flash burning molding method for preparing of ceramic powder stock, are original with ceramic powders
The direct flash burning equipment design scheme of material, it, which does not need to advance with dry-pressing, isostatic cool pressing or the tape casting, prepares ceramic green, because
And significantly simplified Ceramic Production process, using with refractory ceramics and graphite as mold materials can be more accurate control
Shape of product processed and size, so that flash burning technology be made to have the bases of industrial applications.
Technical solution is as follows:
A kind of direct flash burning molding method for preparing of ceramic powder stock, steps are as follows:
(1) raw material is poured into mold, vibration makes its surfacing；
(2) mold is put into ceramic powder stock straight forming flash burning equipment, applies 40 ~ 50MPa pressure, keep ceramic powders former
Material is in heating zone middle position；
(3) auxiliary heating power supply (being herein induction heating power) is opened, is heated to 100 DEG C/min ~ 110 DEG C/min speed
900 DEG C ~ 1000 DEG C or until generation phosphere；
(4) high voltage direct current flash burning power supply is opened, in sample two sides and passes to direct current, linearly increasing voltage about 200V/cm, until
Phosphere occurs；
(5) control electric current is down to 1000A hereinafter, constant current；Continue 20~50s；
(6) it is cooled to room temperature, obtains fine and close sintered body；
(7) sintered body is polished directly, obtains required product.
Further, in step (1), raw material is compound zirconia pelletizing or mixed rare-earth oxide pelletizing.
Further, mixed rare-earth oxide pelletizing is for luteium oxide, gadolinium oxide, europium oxide by mixing, wherein oxygen
Change lutetium content is 70~90mol%, and oxidation gadolinium concentrations are 10~20mol%, and europium oxide content is 0~10mol%.
Further, the ingredient of compound zirconia pelletizing be yttria-stabilized zirconia, wherein yttria levels be 3~
12%mol, aluminum oxide content are 0~66 %mol.
Further, ceramic powder stock straight forming flash burning equipment includes pressurizing device, vacuum chamber, auxiliary heating electricity
Source, high voltage direct current flash burning power supply, control system, cooling system；Raw material, which is placed in the mold of refractory ceramics and graphite composition, to be located at
Internal vacuum chamber center, by compression system pressure confines；Auxiliary heating power supply enters internal vacuum chamber by outer vacuum chamber wall and adds
Thermal Ceramics powder raw material；High voltage direct current flash burning power supply is applied by the water cooling copper electrode at push-down head on pressurizing device to graphite jig
Making alive；
In use, preheating required temperature before providing flash burning by the heater of auxiliary heating system for ceramic powder stock sintering
Degree, while applying certain pressure by pressurizing device；After temperature reaches setting value, applied by high voltage direct current flash burning power supply straight
Galvanic electricity field forms flash burning, realizes the low temperature quick densifying of ceramic material；High voltage direct current flash burning power supply can by process control,
It is transferred to current control from voltage control when flash burning occurs, terminates heating after certain time, is then cooled to room temperature.
Further, mold is nearby equipped with the temperature-detecting device for measuring sample temperature in the vacuum chamber, low
In 1600 DEG C, thermocouple is can be selected in temperature-detecting device；Temperature data input control system, for control auxiliary heating power supply with
And the Current Voltage parameter of flash burning power supply；So that sample realizes stable heat-agglomerating.
Further, when being higher than 1600 DEG C, it is also possible to which infrared radiation thermometer replaces thermocouple to realize temperature measurement.
Compared with prior art, using ceramic powders as the direct flash burning equipment design scheme of raw material, it is not needed the present invention
It advances with dry-pressing, isostatic cool pressing or the tape casting and prepares ceramic green, thus significantly simplified Ceramic Production process, use
Shape of product and size can be more precisely controlled as mold materials with refractory ceramics and graphite, so that flash burning technology be made to have
For the basis of industrial applications.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention.
Specific embodiment
Embodiment 1:
Referring to Fig. 1, the present embodiment shows a kind of ceramic powder stock straight forming flash burning equipment, including pressurizing device 1, vacuum
Room 3, auxiliary heating power supply 6, high voltage direct current flash burning power supply 4, control system 5, cooling system 7 form.
Sample powder, which is placed in the mold of refractory ceramics and graphite composition, is located at internal vacuum chamber center, by compression system pressure
Force constraint.
Heating power supply is assisted to enter internal vacuum chamber heating ceramic powder raw material by outer vacuum chamber wall.
High voltage direct current flash burning power supply applies voltage to graphite jig by the water cooling copper electrode at push-down head on pressurizing device.
In use, being that ceramic powder stock sintering is provided before flash burning needed for preheating by the heater of auxiliary heating system
Temperature, while applying certain pressure by pressurizing device；After temperature reaches setting value, applied by high voltage direct current flash burning power supply 4
Add DC electric field to form flash burning, realizes the low temperature quick densifying of ceramic material；High voltage direct current flash burning power supply 4 can pass through program
Control is transferred to current control from voltage control when flash burning occurs, terminates heating after certain time, be then cooled to room
Temperature.
Mold is nearby equipped with the temperature-detecting device for measuring sample temperature in the vacuum chamber 3, is being lower than 1600 DEG C
When, thermocouple, temperature data input control system, for controlling auxiliary heating power supply and flash burning can be selected in temperature-detecting device
The Current Voltage parameter of power supply.So that sample realizes stable heat-agglomerating.
When being higher than 1600 DEG C, it is also possible to which infrared radiation thermometer replaces thermocouple to realize temperature measurement.
Wherein: the ceramic powder stock straight forming flash burning equipment of the present embodiment can be composed vacuum system, pressure system
System, auxiliary heating system and high voltage direct current flash burning power-supply system and its observing and controlling and cooling system:
(1) vacuum system: since push-down head (having both electrode function) uses graphite material on mold, and it is in the stone of the condition of high temperature
Ink can aoxidize in air, so the heating part of device needs to be maintained in vacuum or inert gas shielding.In the device
The heart proposes a set of vacuum chamber of meter, configures heatshield material, and up and down and surrounding designs connecting flange, be used for electrode, water cooled pipeline and
The access of bonding press.Vacuum chamber is vacuumized, cold conditions ultimate vacuum reaches 10Pa or less by pipeline with a vacuum pump.Simultaneously
Air charging system is designed, nitrogen can be filled with as inert gas shielding, hydrogen can also be poured and form reducing atmosphere.
(2) pressure system:
It can be used hydraulic press, electric press, mechanical press or electro-hydraulic servo press as pressure system.Rated pressure optional 1 ~
250 tons.Dwell time is greater than ten minutes.Press upper pressure head accesses vacuum by seal bellows flange or other dynamic sealing modes
Interior, by 99 alumina ceramic plates and electrode insulation, the cold copper electrode of lower accepting water constitutes pressure system together with graphite jig.
Graphite jig is made of high-purity hot isostatic pressing graphite is machined, is divided into upper die and lower die, external mold insulation pottery
Porcelain aluminium oxide, boron nitride or silicon carbide production.Internal cavity is designed as 12 ~ 180mm of Φ, surface polishing.
(3) heating system
Heating system is made of resistance heating or induction heating power, accesses vacuum chamber by flange.Heater combination thermal insulating material
Material package refractory ceramics former.Centre insertion thermocouple is for measuring and controlling temperature.About 10 ~ 200 kilowatts of power.Operating temperature
It is 400 ~ 1000 DEG C.
(4) power-supply system
Programme-controlled dc power is selected to carry out electric field controls first, power supply accesses vacuum chamber by electrode flange, is connected to push-down head
On the water cooling copper electrode of design, it is connected with graphite electrode, thus builds the high-voltage dc by ceramic powder.
(5) furthermore device further includes the attachmentes such as cabinet, control platform, water cooling unit, for guaranteeing that system can be safe and efficient
Operation.
Embodiment 2:
The sintering of tabular zirconia ceramics is carried out using the ceramic powder stock straight forming flash burning equipment that embodiment 1 is shown,
Steps are as follows:
(1) compound zirconia pelletizing is poured into mold, vibration makes its surfacing；
(2) mold is put into present device, applies 50MPa pressure, ceramic powder stock is made to be in heating zone middle position；
(3) auxiliary heating power supply (being herein induction heating power) is opened, is heated to 1000 DEG C with the speed of 100 DEG C/min；
(4) high voltage direct current flash burning power supply is opened, in sample two sides and passes to direct current, linearly increasing voltage about 100V/cm, until
Phosphere occurs, switchs to current control, rapidly with 100mA/mm2Electric current sintering 2min, fine and close burning can be obtained by being cooled to room temperature
Knot body.
The ingredient of compound zirconia pelletizing is yttria-stabilized zirconia in the step (1), wherein yttria levels
For 3~12%mol, aluminum oxide content is 0~66 %mol.
The density of the present embodiment preparation gained zirconia ceramics sintered body is measured using Archimedes method, and averag density is reachable
The 99.5% of theoretical density, no microscopic holes defect, measures using three-point bending method, and bending strength is greater than 850 MPa, using pressure
Trace method measures fracture toughness and is greater than 7 Mpam1/2, it is micro- less than 1 that visible average grain size is observed using scanning electron microscope
Rice, mechanical property are suitable with high temperature sintering technique products obtained therefrom；The technique combines solid-phase sintering and flash burning technology, is used
Solid phase sintering temperature it is 400 DEG C lower than hot pressing and sintering technique, and be sintered total time be no more than 20 minutes, have process control, system
Standby efficiently and more energy saving advantage, is suitable for industrialized production.
Embodiment 3:
Rare earth oxide transparent ceramic scintillator is carried out using the ceramic powder stock straight forming flash burning equipment that embodiment 1 is shown
Sintering, steps are as follows:
(1) by mixed rare-earth oxide pelletizing (ingredient is luteium oxide, gadolinium oxide, europium oxide, wherein luteium oxide content be 70~
90mol%, oxidation gadolinium concentrations are 10~20mol%, and europium oxide content is 0~10mol%) it pours into mold, oscillation keeps its smooth；
(2) mold is put into present device, applies 40MPa pressure, ceramic powder stock is made to be in heating zone middle position；
(3) auxiliary heating power supply (being herein induction heating power) is opened, is heated to 900 DEG C with the speed of 100 DEG C/min；
(4) high voltage direct current flash burning power supply is opened, in sample two sides and passes to direct current, linearly increasing voltage about 200V/cm, until
Phosphere occurs；
(5) control electric current is down to 1000A hereinafter, constant current；Continue 20~50s；
(6) it is cooled to room temperature, obtains rare earth oxide transparent ceramic scintillator dense sintering body；
(7) sintered body is polished directly, forms transparent ceramic scintillator product.
The present embodiment can not only provide the transparent ceramic scintillator for meeting high-energy X-ray radiation detection application, make simultaneously
It is standby that speed is fast, transparency is high, at low cost.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these belong to protection model of the invention
It encloses.
Claims (7)
1. a kind of direct flash burning molding method for preparing of ceramic powder stock, it is characterised in that: steps are as follows:
(1) raw material is poured into mold, vibration makes its surfacing；
(2) mold is put into ceramic powder stock straight forming flash burning equipment, applies 40 ~ 50MPa pressure, keep ceramic powders former
Material is in heating zone middle position；
(3) auxiliary heating power supply (being herein induction heating power) is opened, is heated to 100 DEG C/min ~ 110 DEG C/min speed
900 DEG C ~ 1000 DEG C or until generation phosphere；
(4) high voltage direct current flash burning power supply is opened, in sample two sides and passes to direct current, linearly increasing voltage about 200V/cm, until
Phosphere occurs；
(5) control electric current is down to 1000A hereinafter, constant current；Continue 20~50s；
(6) it is cooled to room temperature, obtains fine and close sintered body；
(7) sintered body is polished directly, obtains required product.
2. the direct flash burning molding method for preparing of a kind of ceramic powder stock according to claim 1, it is characterised in that: step
(1) in, raw material is compound zirconia pelletizing or mixed rare-earth oxide pelletizing.
3. the direct flash burning molding method for preparing of a kind of ceramic powder stock according to claim 2, it is characterised in that: mixing
Rare earth oxide pelletizing for luteium oxide, gadolinium oxide, europium oxide by mixing, and wherein luteium oxide content is 70~90mol%,
Oxidation gadolinium concentrations are 10~20mol%, and europium oxide content is 0~10mol%.
4. the direct flash burning molding method for preparing of a kind of ceramic powder stock according to claim 2, it is characterised in that: compound
The ingredient of zirconium oxide pelletizing is yttria-stabilized zirconia, and wherein yttria levels are 3~12%mol, and aluminum oxide contains
Amount is 0~66 %mol.
5. the direct flash burning molding method for preparing of a kind of ceramic powder stock according to claim 3 or 4, it is characterised in that:
Ceramic powder stock straight forming flash burning equipment includes pressurizing device, vacuum chamber, auxiliary heating power supply, high voltage direct current flash burning electricity
Source, control system, cooling system；Raw material, which is placed in the mold of refractory ceramics and graphite composition, is located at internal vacuum chamber center, by
Compression system pressure confines；Heating power supply is assisted to enter internal vacuum chamber heating ceramic powder raw material by outer vacuum chamber wall；It is high
Straightening stream flash burning power supply applies voltage to graphite jig by the water cooling copper electrode at push-down head on pressurizing device；
In use, preheating required temperature before providing flash burning by the heater of auxiliary heating system for ceramic powder stock sintering
Degree, while applying certain pressure by pressurizing device；After temperature reaches setting value, applied by high voltage direct current flash burning power supply straight
Galvanic electricity field forms flash burning, realizes the low temperature quick densifying of ceramic material；High voltage direct current flash burning power supply can by process control,
It is transferred to current control from voltage control when flash burning occurs, terminates heating after certain time, is then cooled to room temperature.
6. the direct flash burning molding method for preparing of a kind of ceramic powder stock according to claim 5, it is characterised in that: described
Mold is nearby equipped with the temperature-detecting device for measuring sample temperature in vacuum chamber, is being lower than 1600 DEG C, temperature-detecting device
Thermocouple can be selected；Temperature data input control system, for controlling the Current Voltage of auxiliary heating power supply and flash burning power supply
Parameter；So that sample realizes stable heat-agglomerating.
7. the direct flash burning molding method for preparing of a kind of ceramic powder stock according to claim 6, it is characterised in that: in height
When 1600 DEG C, it is also possible to which infrared radiation thermometer replaces thermocouple to realize temperature measurement.
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| CN114988900A (en) * | 2022-04-27 | 2022-09-02 | 郑州大学 | Method for preparing whisker toughened ceramic matrix composite material by dynamic pressure flash firing |
| CN116514558A (en) * | 2023-04-28 | 2023-08-01 | 西安交通大学 | Ceramic room temperature flash firing system and method |
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