CN109357528A - A kind of ceramic material sintering furnace and its control method using electric field-assisted - Google Patents
A kind of ceramic material sintering furnace and its control method using electric field-assisted Download PDFInfo
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- CN109357528A CN109357528A CN201810921063.9A CN201810921063A CN109357528A CN 109357528 A CN109357528 A CN 109357528A CN 201810921063 A CN201810921063 A CN 201810921063A CN 109357528 A CN109357528 A CN 109357528A
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Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
- F27B17/0016—Chamber type furnaces
- F27B17/0041—Chamber type furnaces specially adapted for burning bricks or pottery
- F27B17/0075—Heating devices therefor
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- 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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D11/00—Arrangement of elements for electric heating in or on furnaces
- F27D11/12—Arrangement of elements for electric heating in or on furnaces with electromagnetic fields acting directly on the material being heated
-
- 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
- F27D19/00—Arrangements of controlling devices
-
- 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
- F27D19/00—Arrangements of controlling devices
- F27D2019/0028—Regulation
- F27D2019/0034—Regulation through control of a heating quantity such as fuel, oxidant or intensity of current
- F27D2019/0037—Quantity of electric current
Abstract
The present invention provides a kind of ceramic material sintering furnaces and its control method using electric field-assisted, including tube furnace, clamping device, electric field to apply module and data observation and logging modle；The clamping device includes two tube bodies, and two tube body both ends seal, and are separately positioned in the both ends of tube furnace by corresponding support device；Two opposite one end of tube body are respectively arranged with electrode；One of electrode, data observation applies module with logging modle, electric field and another electrode passes sequentially through conducting wire and connects.It is that the tube body with conduct piece is provided with inside the both ends of traditional tube furnace.During the sintering process, the sintering densification process of ceramic material can be greatly promoted by applying external electrical field, to realize the low temperature flash burning of ceramic material, i.e., realize the densification of ceramic material in tens seconds time at low temperature.It is final to reduce ceramic sintering temperature, shorten the ceramic post sintering time, greatly saves energy loss.
Description
Technical field
The invention belongs to ceramic post sintering preparation technical fields, are related to sintering furnace, and in particular to a kind of using electric field-assisted
Ceramic material sintering furnace and its control method.
Background technique
Sintering furnace be it is a kind of at high temperature, generate ceramic green solid particle mutually bonded, crystal grain is grown up, and stomata subtracts
Few, total volume is shunk, and density increases, and finally becomes the stove with certain microstructural dense multicrystalline sintered body.
Currently, often utilizing external heat source, such as resistance wire when preparing ceramic material using conventional sintering furnace to be sintered
Deng being heated by way of thermal convection, however these modes need hot conditions and prolonged isothermal holding, this sintering
Energy consumption is high for furnace, and sintered ceramic material is at high cost.
Summary of the invention
Existing shortcoming in view of the prior art, the object of the present invention is to provide a kind of using electric field-assisted
Ceramic material sintering furnace and its control method solve the high energy consumption that conventional ceramic sintering furnace sintering temperature is high, sintering time is long
Problem.
In order to solve the above-mentioned technical problem, the application, which adopts the following technical scheme that, is achieved:
A kind of ceramic material sintering furnace using electric field-assisted, including tube furnace, clamping device, electric field apply module sum number
According to observation and logging modle；The clamping device includes two tube bodies, and two tube body both ends seal, and pass through corresponding branch
Support arrangement is separately positioned in the both ends of tube furnace；Two opposite one end of tube body are respectively arranged with electrode；One of electrode,
Data observation applies module with logging modle, electric field and another electrode passes sequentially through conducting wire and connects.
Further, the recess that the phase proximal end of two sections of tube bodies is respectively equipped with a protrusion and matches with the protrusion
Electrode is respectively equipped on the opposite face of portion, the protrusion and recessed portion.
Further, the conducting wire passes through tube body and connects with corresponding electrode.
Further, the tube body is the step-like tube body for including the first pipeline section and the second pipeline section, wherein first pipe
The caliber of section is less than the second pipeline section；First pipeline section is connected with support device and is set with spring thereon；The both ends of the spring
It is withstood on support device and the second pipeline section respectively.
Further, the support device includes support frame and pulley, and support frame as described above is arranged in the lower section of tube body, and with
The spring contact；The pulley is mounted on support frame bottom, and pulley is equipped with lock.
Further, an additional circuit protection mould is in series between the data observation and logging modle and clamping device
Block.
The present invention also protects a kind of control method of ceramic material sintering furnace using electric field-assisted, and this method is using as above
The ceramic material sintering furnace using electric field-assisted.
Method includes the following steps:
Step 1: in coating platinum slurry in sample two sides to be processed；
Step 2: sample to be processed is placed in the furnace chamber of tube furnace, and is being separately connected electrode for processed sample two sides,
One of electrode, data observation and logging modle are sequentially connected in series using conducting wire, electric field applies module and another electrode；
Step 3: the final temperature that furnace body is arranged is 500~1400 DEG C, and heating rate is 1~20 DEG C/min, setting heat preservation
Time is 2s~30min；
Step 4: the voltage that application is arranged is 1320V, and greatest limit electric current is 100mA；
Step 5: starting tube furnace simultaneously starts electric field application module；
Step 6: curent change situation being observed by data observation and logging modle, when the carrying current set occurs in electric current
When value, keep the temperature in this state；Tube furnace is closed after heat preservation and electric field applies module.
Further, step 3 setting furnace body maximum temperature is 584 DEG C, 750 DEG C, 800 DEG C and 1400 DEG C.
Compared with prior art, there are following advantages by the present invention:
(I) the ceramic material sintering furnace of the invention using electric field-assisted, is set inside the both ends of traditional tube furnace
The tube body with conduct piece is set.When in use, sample to be processed is clamped between the conduct piece of two tube bodies, is then arranged
Sintering temperature, voltage and current parameter after starting electric field applies module, are applied with certain direct current or exchange for sample both ends
Electric field is carried out assisted sintering by the extra electric field, while monitoring sintering process in real time by data observation and logging modle
In Current Voltage variation.During the sintering process, apply external electrical field can be greatly promoted the sintering densification of ceramic material into
Journey realizes the densification of ceramic material to realize the low temperature flash burning of ceramic material at low temperature in tens seconds time.Most
The low ceramic sintering temperature of final decline shortens the ceramic post sintering time, greatly saves energy loss.
(II) recessed portion that the phase proximal end of two sections of tube bodies is respectively equipped with a protrusion and matches with the protrusion, should
So that putting for sample to be processed is more easier, clamping is more stable, while also ensuring the connection of entire circuit for design.
(III) support frame as described above has pulley, and pulley is equipped with lock, so that operator is light when handling sample
Movable supporting frame, after the completion of handling, lock, which can lock pulley, moves support frame not.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the ceramic material sintering furnace of the invention using electric field-assisted.
Fig. 2 is the side view of the alumina ceramic tube of sample clamping device.
Fig. 3 is the main view of the alumina ceramic tube of sample clamping device.
Fig. 4 is prepared the SEM photograph of PZT ceramics by sintering under 1000V voltage.
Fig. 5 is by sintering preparation Al under 1400V voltage2O3The SEM photograph of ceramics.
Fig. 6 is prepared the SEM photograph of KNN ceramics by sintering under 1400V voltage.
Fig. 7 is by sintering preparation ZrO under 1320V voltage2The SEM photograph of ceramics.
Each label is meant that in figure: 1- tube furnace, 2- clamping device, 3- electric field apply module, 4- data observation and note
Record module, 5- support device, 6- electrode, 7- conducting wire, 8- spring, 9- additional circuit protective module；21- tube body, 22- protrusion,
23- recessed portion, 51- support frame, 52- pulley.
Specific embodiment
The following provides a specific embodiment of the present invention, it should be noted that the invention is not limited to implement in detail below
Example, all equivalent transformations made on the basis of the technical solutions of the present application each fall within protection scope of the present invention.
It should be noted that in the absence of explanation to the contrary, the noun of locality used such as " upper and lower " is typically referred to phase
It answers and defines on the basis of the drawing of attached drawing.
In compliance with the above technical solution, as shown in Fig. 1 to Fig. 3, a kind of ceramic material sintering furnace using electric field-assisted, including
Tube furnace 1, clamping device 2, electric field apply module 3 and data observation and logging modle 4；The clamping device 2 includes two pipes
Body 21, two 21 both ends of tube body sealings, and be separately positioned in the both ends of tube furnace 1 by corresponding support device 5；Two
The opposite one end of a tube body 21 is respectively arranged with electrode 6；One of electrode 6, data observation and logging modle 4, electric field apply
Module 3 and another electrode 6 pass sequentially through the series connection of conducting wire 7.
Ceramic material sintering furnace using electric field-assisted of the invention is arranged inside the both ends of traditional tube furnace 1
Tube body 21 with conduct piece.When in use, sample to be processed is clamped between the conduct piece of two tube bodies 21, is then set
Set sintering temperature, voltage and current parameter, after starting electric field applies module 3, for sample both ends be applied with certain direct current or
AC field is carried out assisted sintering by the extra electric field, while being sintered by data observation and the real time monitoring of logging modle 4
Current Voltage variation in the process.During the sintering process, apply the densified sintering product that external electrical field can be greatly promoted ceramic material
Change process realizes the densification of ceramic material to realize the low temperature flash burning of ceramic material at low temperature in tens seconds time
Change.It is final to reduce ceramic sintering temperature, shorten the ceramic post sintering time, greatly saves energy loss.
Specifically, the electric field applies the direct current or AC power source that module 3 can be controllable using a voltage and current, with
It is accurately controlled output voltage and electric current, voltage range can be in 0-2000mA in 0-2000V, current range.
Specifically, the data observation and logging modle 4 can accurately measure the Parameters variations such as Current Voltage in circuit for one
Multimeter, the Current Voltage variation in Observable sintering process.The data observation and logging modle pass through to these data
The detection of variation, it can be achieved that monitoring to actually applied electric field level on sample in sintering furnace, by current change rate and
The observation of variation degree, it can be seen that whether have the generation of Fast Sintering densification behavior, and sintering degree is judged.
Specifically, the phase proximal end of two sections of tube bodies 21 is respectively equipped with a protrusion 22 and matches with the protrusion 22
Electrode 6 is respectively equipped on recessed portion 23, the protrusion 22 and the opposite face of recessed portion 23.In use, sample is placed on recessed
In concave portion 23, protrusion 22 is then protruded into recessed portion 23 and withstands sample.The design of protrusion 22 and recessed portion 23 is so as to be added
Putting for work sample is more easier, while also ensuring the connection of entire circuit.
Preferably, the conducting wire 7 passes through tube body 21 and connects with corresponding electrode 6；The hollow space of tube body 21 both saves material
Material facilitates conducting wire 7 to pass through 21 connection electrode 6 of tube body again.It is furthermore preferred that platinized platinum and platinum filament is respectively adopted in electrode and conducting wire, it is resistant to furnace
Intracavitary high temperature and oxidation resistance is strong.
Preferably, the tube body 21 is the step-like tube body for including the first pipeline section and the second pipeline section, wherein first pipe
The caliber of section is less than the second pipeline section；First pipeline section is connected with support device 5 and is set with spring 8 thereon；The two of the spring 8
End is withstood on respectively on support device 5 and the second pipeline section.It may be implemented to be continuously applied pressure to sample by the elastic force of spring 8,
Guarantee that in test entire circuit is in channel status.It is furthermore preferred that guaranteeing that the elastic force of spring gives sample when selecting spring 8
Pressure range be 10-500Pa.
Specifically, the support device 5 includes support frame 51 and pulley 82, support frame as described above 51 is arranged under tube body 21
Side, and contacted with the spring 8；The pulley 82 is mounted on 51 bottom of support frame, and pulley 82 is equipped with lock.Pulley 52
So that operator's light movable supporting frame when handling sample, after the completion of handling, lock, which can lock pulley 52, makes support frame
51 do not move.
Specifically, being in series with an additional circuit protection mould between the data observation and logging modle 4 and clamping device 2
Block 9 can be avoided and occur that punch-through electric current is excessive to burn power supply during ceramic post sintering.Preferably, additional circuit protects mould
Block 9 is a slide rheostat, and Standard resistance range is 0-500 ohm.
Specific steps are as follows:
Step 1: preparing sample to be processed, and in two sides coating platinum slurry.
Step 2: sample to be processed being pushed into the furnace chamber of tube furnace 1, and be separately connected electrode for processed sample two sides
6, one of electrode 6, data observation and logging modle 4 are sequentially connected in series using conducting wire 7, electric field applies module 3 and another electricity
Pole 6.
Step 3: for setting furnace body maximum temperature between 500 to 1500 DEG C, heating rate is 10 DEG C/min, and corresponding setting is protected
The warm time.
Step 4: the voltage of application being set between 1000V to 1400V, greatest limit electric current is 100mA, and electric field applies mould
Block 3, and start tube furnace 1.
Step 5: observation curent change situation maintains to keep 2s in this state when the limiting value set occurs in electric current
To 30 minutes, it is then shut off sintering equipment.
Explanation is further explained to above scheme below in conjunction with specific embodiment.
Embodiment 1:
The present embodiment provides a kind of ceramic material sintering furnace using electric field-assisted, including tube furnace 1, is externally provided with shell,
Having time and Control for Kiln Temperature unit on shell can realize the pre- of tubular type furnace body temperature program by time and Control for Kiln Temperature unit
If the PZT ceramic powder single shaft prepared is pressed into cylindric, it is stand-by that both ends of the surface coat platinum slurry.The PZT pottery for coating platinum slurry
Porcelain sample is placed on the front end of the alumina ceramic tube 2 of side, and front end is equipped with a platinized platinum 6, sample is gently sticked on platinized platinum 6, platinum filament 7
It is connected across ceramic tube 2 with platinized platinum 6, the other end stretches out ceramic tube 2, and spring 8 is placed between ceramic tube 2 and support frame 51, one end
It is against on the step of ceramic tube 2, the other end resists support frame 51, and the pulley 82 of belt lock catch is arranged at the bottom of support frame 51.By sample
After placing, both sides support frame 51,22 He of protrusion to match by the elastic force and 2 front end of ceramic tube of spring 8 are slowly pushed
The contact that sample is clamped in center and keeps electrode stable by recessed portion 23.Additional circuit protective device 9 is placed in outside, and access is closed
Suitable 200 Ω of protective resistance is powered on the right side of line protection device 9, access data observation and logging modle 4 outside, sees in data
The right side of device 9 is surveyed, accesses electric field bringing device 3, then the circuit both ends connected are stretched with from two sides ceramic tube 2 respectively
Platinum filament 7 be connected, complete the connection of entire circuit.
When work, the setting of temperature program is completed by time and temperature control unit 3.Setting initial temperature is room temperature,
Heating rate is 10 DEG C/min.The setting that voltage and maximum current output parameter are carried out by electric field bringing device 3, wherein exporting
Voltage is 1000V, carrying current 100mA, starts tube furnace 1 and electric field bringing device 3 after being provided with, and realizes and makes pottery to PZT
The electric field-assisted of porcelain sample is sintered.Pay attention to observing the registration in data observation and logging modle 4 when sintering, when furnace temperature is 500 DEG C
When, electric current quickly increases the electric current that reaches capacity, and keeps sintering 30s in this state, is then shut off sintering equipment.Fig. 4 is this
Part is lower to be sintered the SEM photograph for preparing PZT, it can be seen that sample realizes complete densification.Come compared to conventional sintering mode
It says, using sintering furnace provided by the present invention, the sintering temperature of PZT ceramic material reduces 400 DEG C or so, and sintering time is from several
Hour is reduced to 30s.
Embodiment 2:
The present embodiment provides a kind of ceramic material sintering furnace using electric field-assisted, the difference of the present embodiment and embodiment 1
It is only that, sample to be processed uses Al2O3Ceramic material, it is 1400V, final furnace that applied voltage, which is arranged, by electric field bringing device 3
Temperature is 1400 DEG C.
Fig. 5 is is sintered preparation Al under this condition2O3The SEM photograph of ceramics, it can be seen that sample realizes complete densification
Change.For conventional sintering mode, using sintering furnace provided by the present invention, Al2O3The sintering temperature of ceramic material reduces
300 DEG C or so, sintering time is reduced to 30s from a few houres.
Embodiment 3:
The present embodiment provides a kind of ceramic material sintering furnace using electric field-assisted, the difference of the present embodiment and embodiment 1
It is only that, sample to be processed uses KNN ceramic material, and it is 1400V, final furnace that applied voltage, which is arranged, by electric field bringing device 3
Temperature is 750 DEG C.
Fig. 6 by under this condition sintering prepare the SEM photographs of KNN ceramics, it can be seen that sample realizes complete densification
Change.For conventional sintering mode, using sintering furnace provided by the present invention, the sintering temperature of KNN ceramic material is reduced
300 DEG C or so, sintering time is reduced to 30s from a few houres.
Embodiment 4:
The present embodiment provides a kind of ceramic material sintering furnace using electric field-assisted, the difference of the present embodiment and embodiment 1
It is only that, sample to be processed uses ZrO2 ceramic material, and it is 1320V, final furnace that applied voltage, which is arranged, by electric field bringing device 3
Temperature is 800 DEG C.
Fig. 7 by under this condition sintering prepare the SEM photographs of ZrO2 ceramics, it can be seen that sample almost densifies.
For conventional sintering mode, using sintering furnace provided by the present invention, the sintering temperature of ZrO2 ceramic material reduces 500
DEG C or so, sintering time is reduced to 60s from a few houres.
Claims (9)
1. a kind of ceramic material sintering furnace using electric field-assisted, including tube furnace (1), which is characterized in that further include clamping dress
Set (2), electric field applies module (3) and data observation and logging modle (4)；
The clamping device (2) includes two tube bodies (21), and two tube body (21) both ends seal, and pass through corresponding support
Device (5) is separately positioned in the both ends of tube furnace (1)；
Two opposite one end of tube body (21) are respectively arranged with electrode (6)；One of electrode (6), data observation and record mould
Block (4), electric field apply module (3) and another electrode (6) passes sequentially through conducting wire (7) series connection.
2. utilizing the ceramic material sintering furnace of electric field-assisted as described in claim 1, which is characterized in that two sections of tube bodies
(21) recessed portion (23) that phase proximal end is respectively equipped with a protrusion (22) and matches with the protrusion (22), the protrusion
(22) and electrode (6) are respectively equipped on the opposite face of recessed portion (23).
3. utilizing the ceramic material sintering furnace of electric field-assisted as described in claim 1, which is characterized in that the conducting wire (7) is worn
Tube body (21) is crossed to connect with corresponding electrode (6).
4. utilizing the ceramic material sintering furnace of electric field-assisted as described in claim 1, which is characterized in that the tube body (21) is
Step-like tube body including the first pipeline section and the second pipeline section, wherein the caliber of first pipeline section is less than the second pipeline section；First pipe
Section is connected with support device (5) and is set with spring (8) thereon；The both ends of the spring (8) withstand on support device (5) respectively
And second on pipeline section.
5. utilizing the ceramic material sintering furnace of electric field-assisted as described in claim 1, which is characterized in that the support device
(5) include support frame (51) and pulley (52), support frame as described above (51) is arranged in the lower section of tube body (21), and with the spring
(8) it contacts；The pulley (52) is mounted on support frame (51) bottom, and pulley (52) is equipped with lock.
6. as described in claim 1 utilize electric field-assisted ceramic material sintering furnace, which is characterized in that the data observation with
An additional circuit protective module (9) is in series between logging modle (4) and clamping device (2).
7. a kind of control method of the ceramic material sintering furnace using electric field-assisted, which is characterized in that this method uses such as right
It is required that utilizing the ceramic material sintering furnace of electric field-assisted described in 1 to 6 any claim.
8. utilizing the control method of the ceramic material sintering furnace of electric field-assisted as claimed in claim 7, which is characterized in that this method packet
Include following steps:
Step 1: in coating platinum slurry in sample two sides to be processed；
Step 2: sample to be processed being placed in the furnace chamber of tube furnace (1), and be separately connected electrode for processed sample two sides
(6), one of electrode (6), data observation and logging modle (4) are sequentially connected in series using conducting wire (7), electric field applies module (3)
With another electrode (6)；
Step 3: the final temperature that furnace body is arranged is 500~1400 DEG C, and heating rate is 1~20 DEG C/min, and soaking time is arranged
For 2s~30min；
Step 4: the voltage that application is arranged is 1320V, and greatest limit electric current is 100mA；
Step 5: starting tube furnace (1) simultaneously starts electric field application module (3)；
Step 6: curent change situation being observed by data observation and logging modle (4), when the carrying current set occurs in electric current
When value, keep the temperature in this state；Tube furnace (1) is closed after heat preservation and electric field applies module (3).
9. utilizing the control method of the ceramic material sintering furnace of electric field-assisted as claimed in claim 8, which is characterized in that step 3 is set
Setting furnace body maximum temperature is 584 DEG C, 750 DEG C, 800 DEG C and 1400 DEG C.
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| CN109081691A (en) * | 2018-09-13 | 2018-12-25 | 长安大学 | A kind of tubular ceramic preparation method |
| CN111261935A (en) * | 2020-03-04 | 2020-06-09 | 四川固蜀材料科技有限公司 | Sodium ion conductor solid electrolyte material, preparation method and application |
| CN111423240A (en) * | 2020-04-03 | 2020-07-17 | 清华大学深圳国际研究生院 | Two-stage sintering method for preparing ceramic 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 |
| CN112024892A (en) * | 2020-08-27 | 2020-12-04 | 中南大学 | Method for manufacturing aluminum electrolytic capacitor anode foil by electric field auxiliary sintering |
| CN112683062A (en) * | 2020-12-08 | 2021-04-20 | 国网江西省电力有限公司电力科学研究院 | Ultrafast sintering method and device for ceramic material |
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