CN217236474U - Coil electric induction and plasma-assisted rapid cold sintering ceramic equipment - Google Patents
Coil electric induction and plasma-assisted rapid cold sintering ceramic equipment Download PDFInfo
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- CN217236474U CN217236474U CN202220048904.1U CN202220048904U CN217236474U CN 217236474 U CN217236474 U CN 217236474U CN 202220048904 U CN202220048904 U CN 202220048904U CN 217236474 U CN217236474 U CN 217236474U
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Abstract
The invention relates to coil electric induction and plasma-assisted rapid cold sintering ceramic equipment, belonging to the field of ceramic production equipment. A coil electric induction and plasma auxiliary rapid cold sintering ceramic device comprises an upper hot pressing plate, an upper electrode, a die, a lower electrode and a lower hot pressing plate from top to bottom in sequence; temperature thermocouples are respectively arranged in the upper hot pressing plate and the lower hot pressing plate, and a temperature control device is connected between the upper hot pressing plate and the lower hot pressing plate; the upper electrode and the lower electrode are of flat plate structures, the center of the upper electrode is also provided with a boss, and a high-frequency discharge plasma power supply is connected between the upper electrode and the lower electrode; the die is of a hollow structure, an upper pressing sheet is arranged at the upper end in the die, a lower pressing sheet is arranged at the lower end in the die, and a high-frequency induction heating coil is arranged on the outer surface of the die; and two ends of the high-frequency induction heating coil are connected with a high-frequency alternating current power supply. The device of the invention heats the ceramics by utilizing coil electric induction and plasma-assisted cold sintering to realize densification.
Description
Technical Field
The invention belongs to the field of ceramic production equipment, relates to coil electric induction and plasma-assisted rapid cold sintering ceramic equipment, and particularly relates to a device for rapidly realizing densification of ceramic powder at a low temperature by utilizing electric induction heating and plasma-assisted heating on the basis of cold sintering.
Background
Ceramic sintering is a process for densifying ceramic powder, generally speaking, in many sintering processes, higher temperature (more than 800 ℃) and longer heat preservation time or pressure assistance and the like are needed to densify the ceramic, so as to improve the application performance of the ceramic material. However, the ceramic sintering temperature is too high, so that the processing cost is high, and the preparation of organic, inorganic and metal multi-system composite materials is influenced. Meanwhile, the high temperature causes the problems of uneven heating, serious shrinkage and cracking in the ceramic densification process, and is not beneficial to the sintering preparation of the ceramic. Meanwhile, for co-sintering of multi-material systems, such as organic, inorganic, metal, thin film flexible materials and the like, in a high-temperature sintering process, the problem of mismatched expansion coefficients or incompatibility between physics and chemistry occurs, so that co-sintering of multi-material systems is difficult to realize. In addition, a method of preparing ceramics by cold sintering has been reported, for example: the CN 108137417 a patent combines inorganic compounds, organic compounds, metals, and multi-component composite materials with a solvent to form a mixture, applies a higher pressure to the mixture, and densifies the multi-component composite material at a lower temperature to sinter the composite material. But still has the problems that the sintering time is long and the one-step preparation of many high-temperature ceramics is difficult to realize. Therefore, there is a need for a new apparatus and method for preparing inorganic compounds, organic compounds, metals, multi-component composite materials and high-temperature ceramic densification, which lays a solid foundation for large-scale and high-efficiency preparation and application of multi-component composite materials.
Disclosure of Invention
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
a coil electric induction and plasma auxiliary rapid cold sintering ceramic device comprises an upper hot pressing plate, an upper electrode, a die, a lower electrode and a lower hot pressing plate from top to bottom in sequence; temperature thermocouples are respectively arranged in the upper hot pressing plate and the lower hot pressing plate, and a temperature control device is connected between the upper hot pressing plate and the lower hot pressing plate; the upper electrode and the lower electrode are of flat plate structures, a boss is further arranged in the center of the upper electrode, and a high-frequency discharge plasma power supply is connected between the upper electrode and the lower electrode; the die is of a hollow structure, an upper pressing sheet is arranged at the upper end in the die, a lower pressing sheet is arranged at the lower end in the die, a high-frequency induction heating coil is arranged on the outer surface of the die, and the diameter of the die is consistent with that of the boss; and two ends of the high-frequency induction heating coil are connected with a high-frequency alternating current power supply.
In the above technical solution, further, a sealing chamber is further arranged between the upper electrode and the lower hot pressing plate, and a base is arranged at the lower end inside the sealing chamber; the bottom surface of the lower electrode is fixed at the upper end of the base; the head of the boss is located in the sealed chamber.
In the above technical scheme, further, an air valve is arranged in the base, one side of the air valve is provided with an air hole extending out of the sealing chamber, and the other side of the air valve is connected with the bottom of the mold through a pipeline.
In the above technical scheme, further, insulating pads are arranged between the upper hot pressing plate and the upper electrode and between the lower hot pressing plate and the sealing chamber.
In the above technical solution, further, the mold is cylindrical.
In the above technical solution, further, the high-frequency induction heating coil is a mica heating coil.
Among the above-mentioned technical scheme, further, can also be with temperature thermocouple connection on the heating jacket, the heating jacket sets up in the outside of sealing layer, temperature control device and temperature thermocouple connection.
Compared with the prior art, the invention has the beneficial effects that:
(1) the device of the invention heats the ceramics by utilizing coil electric induction and plasma-assisted cold sintering to realize densification. The device can be modified on the basis of cold sintering equipment, and has the advantages of simple equipment manufacture, high heat conversion efficiency, high temperature rise speed, short heat preservation time, capability of quickly realizing densification at low temperature, low energy consumption, small pollution and the like.
(2) The high-frequency alternating current induction coil is used for carrying out auxiliary heating on the component, so that the instantaneous temperature increase and the rapid densification are facilitated. The discharge plasma is utilized to assist in heating the workpiece, so that the surfaces of ceramic particles in a sintered body are uniformly activated and sintered, local plasma high temperature is realized, and the instant densification effect of ceramic powder can be realized from inside to outside at low temperature.
(3) The preparation method for preparing the inorganic compound, the organic compound, the metal, the multi-component system composite material and the high-temperature ceramic at the low temperature by using the device is simple, and the prepared composite material and the ceramic block have excellent mechanical properties and comprehensive properties and obtain good technical effects.
Drawings
FIG. 1 is a schematic view of the composition of a production apparatus of the present invention.
In the figure, 1, an upper hot pressing plate, 2, an upper electrode, 3, a die, 4, a lower electrode, 5, a lower hot pressing plate, 6, an upper pressing sheet, 7, a lower pressing sheet, 8, an air valve, 9, an insulating pad, 10, a sealing chamber, 11, a temperature measuring thermocouple, 12, a high-frequency induction heating coil, 13, a high-frequency alternating current power supply, 14, a high-frequency plasma power supply and 15 are temperature control devices.
Detailed Description
The treatment process of the present invention is further illustrated below with reference to specific examples.
Example 1
The high-frequency discharge plasma power supply in the embodiment is purchased from a manufacturer: shenzhen, Rongda power technology ltd.
As shown in figure 1, the equipment for rapidly cold sintering ceramic by coil electric induction and plasma assistance sequentially comprises an upper hot pressing plate 1, an upper electrode 2, a die 3, a lower electrode 4 and a lower hot pressing plate 5 from top to bottom. Temperature thermocouples 11 are respectively arranged in the upper hot pressing plate 1 and the lower hot pressing plate 5, and a temperature control device 15 is connected between the upper hot pressing plate and the lower hot pressing plate.
The upper electrode and the lower electrode are of flat plate structures, a boss is further arranged in the center of the upper electrode, and a high-frequency discharge plasma power supply 14 is connected between the upper electrode and the lower electrode. The die 3 is of a cylindrical hollow structure, an upper pressing sheet 6 is arranged at the upper end in the die, a lower pressing sheet 7 is arranged at the lower end in the die, the upper pressing sheet and the lower pressing sheet have a sealing effect, a high-frequency induction heating coil 12 is arranged on the outer surface of the die, and the diameter of the mica heating coil die is consistent with that of the boss. Both ends of the high-frequency induction heating coil 12 are connected to a high-frequency ac power supply 13.
A sealing chamber 10 is further arranged between the upper electrode 2 and the lower hot pressing plate 5, a base is arranged at the lower end in the sealing chamber, the bottom surface of the lower electrode is fixed at the upper end of the base, and the head of the boss is located in the sealing chamber 10. An air valve 8 is arranged in the base, one end of the air valve is provided with an air hole extending out of the sealing chamber, the other end of the air valve is connected with the bottom of the die through a pipeline, and insulating pads 9 are arranged between the upper hot pressing plate 1 and the upper electrode 2 and between the lower hot pressing plate 5 and the sealing chamber 10. The temperature of the hot pressing plate of the temperature control device of the invention can be set to be 300 ℃ for 100-.
In the technical scheme, the temperature thermocouple 11 can be connected to the heating sleeve, the heating sleeve is arranged outside the sealing chamber, and the temperature control device is connected with the temperature thermocouple.
The technology for preparing ceramic by cold sintering directly adopts a hot press machine on the basis of a mould, simultaneously realizes pressurization and heating on the mould, controls the temperature by a temperature controller, and implements high pressure to tightly combine ceramic powder at a lower temperature so as to realize densification.
The method for cold sintering the ceramic by adopting the equipment comprises the following steps: selecting zinc molybdate ceramic powder with the particle size of 100nm-300nm, and wetting the ceramic powder with an acetic acid solution; putting the wetted zinc molybdate powder into a die 3; opening a thermal press machine on an industrial control table, setting the pressure at 30-2000 MPa, pressurizing a die, setting the pressure at 200MPa in the embodiment, opening a heating system on the thermal press machine when the pressure is set, heating the die by utilizing an upper hot pressing plate and a lower hot pressing plate, controlling the heating speed at 5 ℃/min by using a thermocouple 11 and a temperature control device 15, setting the temperature at 150 ℃, and keeping the temperature for 1 h;
when the set temperature is reached, the high-frequency alternating-current power supply 13 is started, and the voltage range is as follows: 50-300V; current range: 10-2000A, realizing coil electric induction auxiliary heating (the instantaneous temperature can reach 800 ℃), starting the high-frequency plasma power supply 14 on the basis, wherein the voltage range is as follows: 50-300V; current range: 10-2000A, the plasma auxiliary heating (the instantaneous temperature can reach 800 ℃) temperature thermocouple 11 sends signals to an industrial control console, and when the temperature measured by the temperature thermocouple reaches the set sintering temperature and the set heat preservation time, the sintering process is finished.
Wherein, the sealing chamber 10: realizing the circulation of vacuum or protective atmosphere; cylindrical mold 3: and the wetted ceramic powder is added into the die cavity to realize ceramic densification.
Wherein, the hot press: pressure forming is realized in the ceramic densification process, and the ceramic powder is compacted by using the pressure of 200MPa, so that the densification of the coating is facilitated;
wherein the hot press machine heats the die, and the temperature is controlled by a temperature control device and is 150 ℃;
wherein, the surface of the mould uses a high-frequency alternating current power supply to provide alternating current for a high-frequency induction heating coil 12, the alternating current flowing through the coil generates an alternating magnetic field, under the action of the magnetic field, induced current with the same frequency as the induction coil or the opposite direction to the induction coil is generated in the ceramic powder, and the magnetic field causes the ceramic powder to generate eddy current for heating (the instantaneous temperature is 800 ℃). The ceramic powder can be rapidly heated, the densification time is shortened, the rapid densification is realized, the time is saved, and the densification is higher than that of single cold-sintered ceramic;
and (4) an air valve 8: the ceramic is used for vacuum pumping or protection of gas-filled atmosphere, auxiliary ceramic forming, further densification of ceramic, or sintering of non-oxide ceramic.
The insulating pad 9 is arranged to prevent current from being guided to the press, so that large current is kept to the maximum extent, and induction heating of the high-frequency induction heating coil is facilitated.
Wherein, a high-frequency discharge plasma power supply 14 is utilized on the die to provide discharge plasma, so that the surfaces of ceramic particles in a sintered body are uniformly activated and sintered, local plasma high temperature is realized, and the ceramic powder is densified from inside to outside (the instantaneous temperature is 800 ℃). Meanwhile, the discharge plasma generates discharge impact pressure and electric field diffusion, and plays a certain role in accelerating ceramic densification. Meanwhile, the ceramic densification can be realized in a short time by combining with the heating of a high-frequency induction coil. The density of the ceramic prepared by the method and the device is more than 90%, and the density testing method is an Archimedes drainage method.
Example 2
The cold sintering equipment and the process method adopted in this embodiment are the same as those in embodiment 1, except that the ceramic powder used in this embodiment is zinc oxide ceramic powder, and the density of the prepared ceramic is more than 90%.
It will be apparent to those skilled in the art from this disclosure that many changes and modifications can be made, or equivalents modified, in the embodiments of the invention without departing from the scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention.
Claims (6)
1. A coil electric induction and plasma auxiliary rapid cold sintering ceramic device is characterized by comprising an upper hot pressing plate, an upper electrode, a die, a lower electrode and a lower hot pressing plate from top to bottom in sequence; temperature thermocouples are respectively arranged in the upper hot pressing plate and the lower hot pressing plate, and a temperature control device is connected between the upper hot pressing plate and the lower hot pressing plate; the upper electrode and the lower electrode are of flat plate structures, the center of the upper electrode is also provided with a boss, and a high-frequency discharge plasma power supply is connected between the upper electrode and the lower electrode; the die is of a hollow structure, an upper pressing sheet is arranged at the upper end in the die, a lower pressing sheet is arranged at the lower end in the die, a high-frequency induction heating coil is arranged on the outer surface of the die, and the diameter of the die is consistent with that of the boss; and two ends of the high-frequency induction heating coil are connected with a high-frequency alternating current power supply.
2. The coil electric induction and plasma auxiliary rapid cold sintering ceramic equipment according to claim 1, wherein a sealed chamber is further arranged between the upper electrode and the lower hot pressing plate, and a base is arranged at the lower end inside the sealed chamber; the bottom surface of the lower electrode is fixed at the upper end of the base; the head of the boss is located in the sealed chamber.
3. The coil electric induction and plasma auxiliary rapid cold sintering ceramic device according to claim 2, wherein an air valve is arranged in the base, one side of the air valve is provided with an air hole extending out of the sealing chamber, and the other side of the air valve is connected with the bottom of the mold through a pipeline.
4. The apparatus of claim 1 wherein insulating spacers are disposed between the upper hot platen and the upper electrode and between the lower hot platen and the seal chamber.
5. The apparatus of claim 1 wherein the die is cylindrical in shape.
6. The apparatus for rapid cold sintering of ceramic by coil induction and plasma-assisted according to claim 1, wherein the high frequency induction heating coil is a mica heating coil.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220048904.1U CN217236474U (en) | 2022-01-10 | 2022-01-10 | Coil electric induction and plasma-assisted rapid cold sintering ceramic equipment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220048904.1U CN217236474U (en) | 2022-01-10 | 2022-01-10 | Coil electric induction and plasma-assisted rapid cold sintering ceramic equipment |
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| CN202220048904.1U Active CN217236474U (en) | 2022-01-10 | 2022-01-10 | Coil electric induction and plasma-assisted rapid cold sintering ceramic equipment |
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