CN116202323A - Ceramic sintering device and ceramic sintering method - Google Patents
Ceramic sintering device and ceramic sintering method Download PDFInfo
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- CN116202323A CN116202323A CN202310262188.6A CN202310262188A CN116202323A CN 116202323 A CN116202323 A CN 116202323A CN 202310262188 A CN202310262188 A CN 202310262188A CN 116202323 A CN116202323 A CN 116202323A
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The application provides a ceramic sintering device and a ceramic sintering method, which are used for sintering ceramic green bodies, wherein the ceramic sintering device comprises a power supply device, a first insulating plate and a second insulating plate, and the first insulating plate is used for supporting the ceramic green bodies; the power supply device is used for providing voltage for the ceramic green body so as to generate an electric arc above the ceramic green body to sinter the ceramic green body; the second insulation board interval sets up on first insulation board, and the second insulation board is used for setting up on the ceramic green compact with predetermineeing the interval, and the second insulation board is used for restraining electric arc in the top of ceramic green compact. In this application, through power supply unit and the both ends electricity of ceramic unburned bricks to provide voltage for ceramic unburned bricks, and produce electric arc in ceramic unburned bricks top, so that ceramic unburned bricks rapidly sinter in the short time under the effect of electric arc, and form densification pottery, thereby realize the sintering to ceramic unburned bricks at room temperature, improve traditional long-time sintered mode.
Description
Technical Field
The application relates to the technical field of ceramic material preparation, in particular to a ceramic sintering device and a ceramic sintering method.
Background
At present, the ceramic material is an inorganic material which is most well seen by people after being used as a metal material and a nonmetal material, has wide application and development prospect, and is an essential key material in modern society and construction development. In the electrical field, dielectric ceramics have been widely used due to their excellent mechanical strength, insulating properties, high temperature resistance, and other characteristics. The manufacture of ceramic materials is still mainly carried out by traditional sintering, the sintering temperature of the traditional sintering process is very high, and the sintering time is relatively long, for example, the sintering temperature of alumina ceramic is as high as 1650-1990 ℃, and the sintering time is required to be several hours. Therefore, the conventional sintering process cannot limit the infinite growth of crystal grains, and the energy loss caused by the conventional sintering mode is huge, so that the energy utilization efficiency is low, and the method for searching for the rapid densification of the ceramic blank is important.
The flash firing is a novel ceramic preparation method and has the advantages of low energy consumption and high sintering speed. However, in view of the current situation, the range of ceramic materials that can be used for flash firing is limited, for example, aluminum oxide ceramic, YSZ ceramic and the like cannot realize flash firing at room temperature at present, and the development and the application of the ceramic are limited.
Disclosure of Invention
In view of this, the present application provides a ceramic sintering apparatus and a ceramic sintering method.
In order to achieve the above object, the present application provides a ceramic sintering device for sintering a ceramic green body, the ceramic sintering device including a power supply device, a first insulating plate for supporting the ceramic green body, and a second insulating plate; the power supply device is used for providing voltage for the ceramic green body so as to generate an electric arc above the ceramic green body to sinter the ceramic green body; the second insulation board interval set up in on the first insulation board, the second insulation board be used for with predetermine interval set up in on the ceramic green compact, the second insulation board be used for with electric arc constraint the top of ceramic green compact.
In some possible implementations, the preset spacing is 2-15 mm.
In some possible implementations, the ceramic sintering device further includes a current limiting resistor device for limiting a current of the power supply device and a voltage-current measuring device for detecting a voltage in the power supply device in real time.
In some possible implementations, the first insulating plate and the second insulating plate each comprise an aluminum oxide ceramic, an aluminum nitride ceramic, or a beryllium nitride ceramic.
In some possible implementations, the power supply device includes a first electrode and a second electrode, the first electrode and the second electrode are respectively connected to two ends of the ceramic green body, and the first electrode and the second electrode respectively use tungsten wires or molybdenum wires.
The application also provides a ceramic sintering method, comprising the following steps: placing a ceramic green body on a first insulating plate, and then arranging a second insulating plate above the first insulating plate at intervals to obtain an intermediate; placing the intermediate in a preset gas atmosphere; and at room temperature, connecting two ends of the ceramic green body with a power supply device, applying voltage to the ceramic green body through the power supply device, and generating an arc above the ceramic green body to sinter the ceramic green body.
In some possible implementations, the current density flowing through the ceramic green body is 75-150 mA/mm 2 The sintering time of the ceramic green body is less than or equal to 2.5 minutes.
In some possible implementations, the thickness of each of the first insulating plate and the second insulating plate is greater than or equal to 1cm.
In some possible implementations, the power supply device has a boost rate of 0.1-5 kV/s.
In some possible implementations, the preset gas atmosphere includes air, oxygen, nitrogen, or argon.
In this application, in ceramic sintering device, through power supply unit and ceramic green compact's both ends electricity connection to provide voltage for ceramic green compact, and produce electric arc in ceramic green compact top, so that ceramic green compact is sintered rapidly in the short time under the effect of electric arc, and form densification ceramic, thereby realize the sintering to ceramic green compact at room temperature, improve traditional long-time sintered mode, reduce the energy consumption of sintering ceramic. Meanwhile, the current flows through the ceramic green body, so that not only can the uniformity of the integral sintering of the ceramic green body be realized, but also the damage of the electric arc to the surface of the ceramic green body can be reduced. In addition, in the power supply device provided by the application, sintering is realized by applying voltage to the ceramic green body and generating electric arc, and the sintering can be completed at room temperature without auxiliary heating of an additional heating device, and the structure is simple. Meanwhile, in the ceramic sintering device provided by the application, the second insulating plates are arranged above the first insulating plates at intervals, so that the electric arc is bound on the surface of the ceramic green body, the efficiency of the electric arc acting on the ceramic green body is improved, and the electric arc is prevented from expanding outwards. The ceramic sintering device provided by the application is simple in structure, easy to operate, applicable to ceramic green bodies made of different materials, high in applicability and beneficial to promoting the development of ceramic flash.
Drawings
Fig. 1 is a schematic structural diagram of a ceramic sintering device according to an embodiment of the present application.
In FIG. 2, (A) is a scanning electron microscope image of the alumina ceramic prepared in example 1, (B) is an X-ray energy spectrum of the alumina ceramic of (A), (C) is an Al element distribution pattern of the alumina ceramic of (A), and (D) is a Zn element distribution pattern of the alumina ceramic of (A).
FIG. 3 is a scanning electron microscope image of YSZ ceramic prepared in example 2.
FIG. 4 is a scanning electron microscope image of the alumina ceramic prepared in the argon atmosphere in example 3.
Fig. 5 is a scanning electron microscope image of the alumina ceramic green body of comparative example 1.
Description of the main reference signs
Wire 13
First insulating plate 20
Second insulating plate 30
Ceramic green body 200
Detailed Description
Embodiments of the present invention are described in detail below. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
Referring to fig. 1, the present embodiment provides a ceramic sintering device 100, wherein the ceramic sintering device 100 includes a power supply device 10, a first insulating plate 20, and a second insulating plate 30, and the first insulating plate 20 may be disposed on a platform (not shown). The ceramic green body 200 is placed on the first insulating plate 20. The second insulating plate 30 is disposed directly above the first insulating plate 20 by a bracket (not shown). The power supply device 10 is electrically connected to both ends of the ceramic green body 200 and supplies a voltage to the ceramic green body 200 to generate an arc above the ceramic green body 200 and sinter the ceramic green body 200, thereby achieving sintering of the ceramic green body 200 at room temperature. In this application, the second insulating plate 30 binds the arc above the ceramic green body 200 such that the arc sinters the entire ceramic green body 200 through the upper surface of the ceramic green body 200.
The second insulating plates 30 are disposed on the ceramic green body 200 at preset interval, and the preset interval between the second insulating plates 30 and the ceramic green body 200 is 2 to 15mm. Under the condition, the ceramic green body 200 can be fully subjected to arc treatment, and the arc can be restrained, so that the arc is prevented from expanding. For example, the spacing may be 2mm, 3mm, 5mm, 7mm, 10mm or 15mm.
In some embodiments, the power supply device 10 includes a power source (not shown), a first electrode 11, a second electrode 12, and a wire 13. The first electrode 11 and the second electrode 12 are connected to a power source through wires 13, respectively. The first electrode 11 and the second electrode 12 are both connected to the ceramic green body 200. Meanwhile, in the above process, it is not necessary to coat both ends of the ceramic green body 200 with conductive silver paste. The first electrode 11 and the second electrode 12 directly realize the electrical connection with the ceramic green body 200 by clamping the ceramic green body 200, thereby simplifying the process steps.
In some embodiments, the first insulating plate 20 and the second insulating plate 30 are made of high-temperature resistant plates, so that the cracking of the first insulating plate 20 and the second insulating plate 30 caused by the electric arc generated by the subsequent ceramic green body 200 is avoided. In some embodiments, the first insulating plate 20 and the second insulating plate 30 are respectively made of aluminum oxide ceramic, aluminum nitride ceramic, or beryllium nitride ceramic. The first insulating plate 20 and the second insulating plate 30 may be made of the same material or different materials. In other embodiments, other high temperature resistant insulating sheets may be used.
In some embodiments, the thickness of both the first insulating plate 20 and the second insulating plate 30 is greater than or equal to 1cm, so as to avoid arcing through the first insulating plate 20 and the second insulating plate 30, causing the first insulating plate 20 and the second insulating plate 30 to burst. In some implementations, the thickness of the first insulating plate 20 and the second insulating plate 30 may be the same or different. For example, the thickness of each of the first insulating plate 20 and the second insulating plate 30 may be 1cm, 2cm, 3cm, 4cm, or 5cm.
In some embodiments, the first electrode 11 and the second electrode 12 are tungsten wires or molybdenum wires, respectively. The melting points of the tungsten wire and the molybdenum wire are higher than 2000 ℃, and the diameters of the first electrode 11 and the second electrode 12 are larger than 0.4mm, so that the first electrode 11 and the second electrode 12 are not fused under high voltage, and the normal operation of the power supply device 10 is ensured.
In some embodiments, the power supply device 10 is further provided with a current limiting resistor device (not shown) and a voltage and current measuring device (not shown), where the current limiting resistor device may be a current limiting resistor, and the voltage and current measuring device may include a voltage and current data acquisition card. The current limiting resistor device is used for limiting the current of the power supply device 10 and protecting the safety of the power supply device 10. The voltage and current measuring device is used for measuring the voltage in the power supply device 10 in real time, and can also adjust the voltage of the whole power supply device 10 according to the requirement, so as to meet the application requirement.
The application also provides a ceramic sintering method, which comprises the following steps:
s1, providing a ceramic green body.
The ceramic green body comprises one of an alumina ceramic green body, a zinc oxide ceramic green body, and a yttrium stabilized zirconia green body.
The specific preparation steps of the ceramic green body comprise: and (3) ball milling the ceramic powder, granulating, grinding the granulated ceramic powder through a 80-mesh screen to obtain final powder, tabletting by a single-shaft press, and discharging glue for 30min at 400 ℃ by a muffle furnace to obtain the ceramic green compact.
S2, placing the ceramic green body on the first insulating plate, and then arranging the second insulating plate right above the first insulating plate at intervals to obtain an intermediate.
In this step, the first insulating plate plays the supporting role to the ceramic green compact, and the second insulating plate interval sets up directly over first insulating plate for in the subsequent handling in-process, restrict the constraint to the electric arc that produces on ceramic green compact surface, avoid electric arc to spread outward, make electric arc can concentrate the surface of acting on ceramic green compact, this on the other hand has also improved the efficiency that electric arc acted on ceramic green compact.
S3, placing the intermediate under a preset gas atmosphere.
The first insulating plate, the second insulating plate and the ceramic green body are simultaneously placed under a preset gas atmosphere. In practical application, different gas atmospheres can be correspondingly selected according to requirements, so that electric arcs are regulated and controlled, the heat energy acting on the ceramic green compact is changed, and the sintering effect of the ceramic green compact is further changed. In some embodiments, the preset gas atmosphere comprises air, oxygen, nitrogen, or argon.
S4, connecting power supply devices at the two ends of the ceramic green body at room temperature, forming a current loop between the power supply devices and the ceramic green body, applying voltage to the ceramic green body through the power supply devices, generating an electric arc above the ceramic green body to sinter the ceramic green body, and sintering the ceramic green body.
In the above steps, the power supply device is arranged at two ends of the ceramic green body, the power supply device provides voltage for the ceramic green body, the two ends of the power supply device and the ceramic green body form a current loop, after the power supply device applies voltage to the ceramic green body, a high-energy electric arc is generated on the surface of the ceramic green body, under the condition of room temperature, the electric arc converts electric energy into heat energy, the electric arc heats the surface of the ceramic green body in a short time, acts on the surface of the ceramic green body and penetrates through the whole ceramic green body, and the ceramic green body is subjected to flash firing. Meanwhile, in the ceramic sintering method provided by the application, current flows through the whole ceramic green body, so that the uniformity of the whole ceramic green body sintering can be realized, and the damage of an electric arc to the surface of the ceramic green body can be reduced.
In some embodiments, the power supply device boosts the voltage at a boost rate of 0.1-5 kV/s until an arc is generated, and the current density flowing through the ceramic green body is 75-150 mA/mm 2 The sintering time of the ceramic green body is less than or equal to 2.5 minutes. In this data range, to ensure that the surface of the ceramic green body can be subjected to high energy arc treatment, while also avoiding excessive time and damage to the power supply device. If the current density is too low, the ceramic green body cannot be ensured to be fast and compact; too high a current density may cause rapid shrinkage of the ceramic green body, resulting in localized overheating and breakage. In some embodiments, the boost rate is 0.1kV/s, 0.2kV/s, 0.5kV/s, 1kV/s, 2kV/s, 3kV/s, or 4kV/s; the current density was 75mA/mm 2 、90mA/mm 2 、100mA/mm 2 、120mA/mm 2 Or 150mA/mm 2 The method comprises the steps of carrying out a first treatment on the surface of the Ceramic materialThe sintering time of the green body is 0.5min, 1min, 1.5min or 2min.
In some embodiments, the power supply device has a rated capacity greater than or equal to 100kVA and a rated output current greater than or equal to 2A. The rated output voltage of the power supply device is 50kV, and the allowable running time is the rated voltage and the current is more than or equal to 30min.
The ceramic comprises one of alumina ceramic, zinc oxide ceramic and yttrium stabilized zirconia. The alumina ceramic is used as the ceramic with the largest application and the largest sales in the current oxide ceramic, and is widely applied to electric network equipment such as electric vacuum devices, device porcelain parts, circuit substrates, thyristors, solid circuit shells and the like. In the field of power industry, alumina ceramics have a wide application foundation due to the remarkable advantages of high mechanical strength, high insulation resistance, low dielectric loss and the like. The ceramic sintering method provided by the application can promote the development of ceramic flash.
The scheme of the present invention will be explained below with reference to examples. It will be appreciated by those skilled in the art that the following examples are for illustrative purposes only and are not to be construed as limiting the invention. Unless otherwise indicated, the reagents, software and instrumentation involved in the examples below are all conventional commercial products or open source.
Example 1
The steps for preparing the alumina ceramic are as follows:
(1) And (3) granulating, ball-milling, tabletting and discharging glue to obtain an alumina ceramic green body containing 5% zinc oxide, wherein the length of the alumina ceramic green body is 14.5mm, the width of the alumina ceramic green body is 3.3mm and the height of the alumina ceramic green body is 1.7mm.
(2) And placing the ceramic green body on the first insulating plate, and tightly contacting with the electrodes at the two sides, so as to keep the power supply in a power-off state. The second insulating plate was placed over the first insulating plate with a 10mm spacing between the green ceramic and the second insulating plate.
(3) And in the normal-pressure air atmosphere, a high-voltage alternating current power supply is turned on, and the voltage is uniformly increased at the speed of 0.2kV/s until high-energy electric arcs are generated to penetrate through the surface of the ceramic green body. At this time, the voltage was adjusted to stabilize the current at 113.5mA/mm 2 And is combined withAfter maintaining for 30s, the power is cut off, and the alumina ceramic is obtained, and the density can reach 97.6%.
Example 2
The yttrium-stabilized zirconia was prepared as follows:
(1) And granulating, ball-milling, tabletting and discharging glue to obtain a 3YSZ ceramic green body, wherein the length of the 3YSZ ceramic green body is 14.5mm, the width of the 3.3mm and the height of the 3YSZ ceramic green body are 1.7mm.
(2) And placing the ceramic green body on a first insulating plate, and tightly contacting with the electrodes at the two sides, so as to keep the power supply in a power-off state. The second insulating plate was placed over the first insulating plate with a 10mm spacing between the green ceramic and the second insulating plate.
(3) And in the normal-pressure air atmosphere, a high-voltage alternating current power supply is turned on, and the voltage is uniformly increased at the speed of 0.2kV/s until high-energy electric arcs are generated to penetrate through the surface of the ceramic green body. At this time, the voltage is regulated to stabilize the current at 90mA/mm 2 And after the ceramic is maintained for 30 seconds, the ceramic is powered off to obtain YSZ ceramic, and the density can reach 99.4%.
Example 3
Example 3 differs from example 1 in that an arc was generated in an argon atmosphere. The remaining steps were the same as in example 1.
Comparative example 1
Comparative example 1 differs from example 1 in that the alumina ceramic green body was not subjected to arc treatment.
The ceramics prepared in examples 1-3 and comparative example 1 were also subjected to scanning electron microscopy.
Referring to fig. 2, (a) is a scanning electron microscope image of the alumina ceramic prepared in example 1, (B) is an X-ray energy spectrum of the alumina ceramic of (a), (C) is an Al element profile in the alumina ceramic of (a), and (D) is a Zn element profile in the alumina ceramic of (a). As can be seen from (a) of fig. 2 described above, the surface of the alumina ceramic after arc sintering is uniform and dense, compared with the green alumina ceramic (see fig. 5) which is not sintered. As can be seen from (B), (C) and (D) in fig. 2, al element and Zn element are distributed on the alumina ceramic surface. Some pores exist on the surface, and the grain size is 9.68+/-0.67 mu m.
Referring to fig. 3, fig. 3 is a scanning electron microscope image of the YSZ ceramic prepared in example 2, and it can be seen from fig. 3 that the YSZ ceramic has a dense surface, substantially no pores, and a grain size of 174.32 ±4.38 μm.
Referring to fig. 4, fig. 4 is a scanning electron microscope image of the alumina ceramic prepared in the argon atmosphere in example 3, and it can be seen from fig. 4 that the surface of the alumina ceramic green body after arc sintering is dense in the argon atmosphere, and the grain size is 1.13±0.35 μm.
The archimedes drainage method test is also carried out on the ceramics prepared in the examples 1-2 and the comparative example 1, and the test shows that the density of the alumina ceramic prepared in the example 1 can reach 97.6 percent compared with the density of an unsintered ceramic green body of 58.3 percent. The density of the YSZ ceramic prepared in the example 2 can reach 99.4 percent. This means that by firing the green ceramic body under the action of an arc, a dense ceramic can be obtained. The alumina ceramic prepared in example 1 meets both the requirements of grid equipment for high performance materials and the requirements of dual carbon development.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. A ceramic sintering device for sintering a ceramic green body, the ceramic sintering device comprising:
a first insulating plate for supporting the ceramic green body;
the power supply device is used for providing voltage for the ceramic green body so as to generate an electric arc above the ceramic green body to sinter the ceramic green body;
the second insulating plate is arranged on the first insulating plate at intervals, the second insulating plate is used for being arranged on the ceramic green body at intervals of preset intervals, and the second insulating plate is used for binding the electric arc above the ceramic green body.
2. The ceramic sintering device according to claim 1, wherein the preset spacing is 2 to 15mm.
3. The ceramic sintering device of claim 1, further comprising a current limiting resistor device for limiting a current of the power supply device and a voltage-current measuring device for detecting a voltage in the power supply device in real time.
4. The ceramic sintering device of claim 1, wherein the first insulating plate and the second insulating plate each comprise an aluminum oxide ceramic, an aluminum nitride ceramic, or a beryllium nitride ceramic.
5. The ceramic sintering device according to claim 1, wherein the power supply device comprises a first electrode and a second electrode, the first electrode and the second electrode are respectively connected to two ends of the ceramic green body, and tungsten wires or molybdenum wires are respectively adopted for the first electrode and the second electrode.
6. A method of sintering ceramic, comprising:
placing a ceramic green body on a first insulating plate, and then arranging a second insulating plate above the first insulating plate at intervals to obtain an intermediate;
placing the intermediate in a preset gas atmosphere;
and at room temperature, connecting two ends of the ceramic green body with a power supply device, applying voltage to the ceramic green body through the power supply device, and generating an arc above the ceramic green body to sinter the ceramic green body.
7. The ceramic sintering method of claim 6, wherein the ceramic green body flows throughThe current density is 75-150 mA/mm 2 The sintering time of the ceramic green body is less than or equal to 2.5 minutes.
8. The ceramic sintering method according to claim 6, wherein the thickness of each of the first insulating plate and the second insulating plate is 1cm or more.
9. The ceramic sintering method according to claim 6, wherein the step-up rate of the power supply device is 0.1 to 5kV/s.
10. The ceramic sintering method according to claim 6, wherein the preset gas atmosphere comprises air, oxygen, nitrogen or argon.
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