CN115650736A - Ceramic room-temperature ultrafast sintering method based on dielectric barrier discharge glue removal treatment - Google Patents
Ceramic room-temperature ultrafast sintering method based on dielectric barrier discharge glue removal treatment Download PDFInfo
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- CN115650736A CN115650736A CN202211236477.0A CN202211236477A CN115650736A CN 115650736 A CN115650736 A CN 115650736A CN 202211236477 A CN202211236477 A CN 202211236477A CN 115650736 A CN115650736 A CN 115650736A
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Abstract
The invention relates to the technical field of ceramic material preparation, and provides a ceramic room temperature ultrafast sintering method based on dielectric barrier discharge glue discharging treatment. Compared with the ceramic green body which is not subjected to binder removal treatment, the room-temperature sintering initial voltage of the ceramic green body subjected to binder removal treatment is reduced by half, and the problem that electric arcs and the like are difficult to control is solved. Compared with the traditional glue discharging device, the glue discharging device provided by the invention has the advantages of short consumed time and low energy consumption, can increase the oxygen defect of the ceramic green body, has lower voltage in the subsequent ultrafast sintering process, and is easier to sinter.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a ceramic room temperature ultrafast sintering method based on dielectric barrier discharge glue removal treatment.
Background
The ceramic material is a non-metal material with a wide application range, and can be used in the scientific and technological advanced fields of electronic instruments, biological medicine, aerospace and the like.
The binder removal is a key link in the ceramic production process, has obvious influence on the performance of the formed ceramic, but the traditional heating binder removal process has the defects of high time consumption, high energy consumption, high pollution and the like, so that the design of a novel rapid and low-energy-consumption binder removal process has important practical significance.
The manufacture of ceramic materials requires high temperatures for a long time to sinter an otherwise relatively loose green body to full density. This means that the conventional ceramic manufacturing process requires a large amount of energy consumption and a long time. In order to reduce the energy consumption in the ceramic sintering process, various novel sintering processes, such as microwave sintering, spark plasma sintering, hot-pressing sintering and the like, are proposed and put into practical use.
The flash firing technology is a novel electric field assisted sintering process appearing in 2010, namely, a proper alternating current or direct current voltage is applied to two ends of a ceramic green body, so that the ceramic green body can be highly densified within seconds to minutes, and the furnace temperature required by ceramic sintering is greatly reduced. Such short sintering times and relatively low furnace temperatures mean that the energy consumption required for flash firing techniques is greatly reduced compared to conventional sintering processes. However, excessive growth of ceramic grains and excessive grain size often occur in the flash firing process, thereby affecting the service performance of the ceramic material. Therefore, the inhibition of the grain growth in the flash combustion process has important significance for further popularization and application of the flash combustion technology.
Disclosure of Invention
The invention aims to overcome at least one of the defects of the prior art and provides a ceramic room temperature ultra-fast sintering method based on dielectric barrier discharge binder removal treatment. The purpose of the invention is realized based on the following technical scheme:
the invention provides a ceramic room temperature ultrafast sintering method based on dielectric barrier discharge glue discharging treatment, which comprises the following steps:
s1, preparing a ceramic green body, wherein the ceramic green body (1) contains a binder;
s2, vertically oppositely arranging two electrode plates, namely, an upper dielectric plate is tightly attached to an upper electrode, a lower dielectric plate is tightly attached to a lower electrode, placing the ceramic green body in the center of the lower dielectric plate, adjusting the distance between the two electrodes, and connecting the two electrodes to a power supply;
s3, setting power supply frequency, increasing the voltage value to a target voltage peak value at a certain boosting rate, maintaining for a period of time after the discharge tends to be stable, and then reducing the voltage and cutting off the power supply to finish the glue discharging process;
s4, spraying electrodes on two ends of the ceramic green body subjected to the glue removing treatment, winding the electrodes at the two ends by using a lead, and connecting the electrodes with a high-voltage power supply through the lead;
and S5, switching on a high-voltage power supply, and adjusting the firing voltage and current to perform room-temperature ultrafast sintering of the ceramic.
Preferably, in step S1, the shape of the ceramic green body includes a cylinder, a rectangular parallelepiped, or a dog-bone shape.
Preferably, in step S1, the adhesive comprises polyvinyl alcohol, and/or polyvinyl acetal Ding Quanzhi.
Preferably, in the step S2, the distance between the upper dielectric plate and the upper surface of the ceramic green body is 1-5mm.
Preferably, in step S3, the power supply frequency is 6-14kHz.
Preferably, the boosting rate in step S3 is 1-4kV/S.
Preferably, the peak-to-peak value of the target voltage in the step S3 is 15-40kV, and the maintaining time is 5-60min.
Preferably, the method of spraying gold or coating conductive silver paste is adopted for the spraying electrodes on the two ends of the processed ceramic green body in step S4, and the wires wound on the electrodes can be metal wires with higher melting points, such as platinum wires.
Preferably, the ceramic green body in step S4 is set in suspension or placed on an insulating ceramic plate.
Preferably, step S5 specifically includes the steps of: and switching on a high-voltage power supply, increasing the amplitude of the voltage until the current flowing through the ceramic green body is suddenly increased and the voltage at two ends of the ceramic green body is suddenly reduced, and switching off the high-voltage power supply after maintaining for a period of time to obtain the ceramic after ultrafast sintering.
Preferably, the high-voltage power supply is an alternating-current power supply or a direct-current power supply, the boosting rate of the boosted voltage is 0.1-1kV/s, and the current density range is 10-150mA/mm 2 。
The invention can obtain at least one of the following beneficial effects:
according to the invention, the reactor is heated by heat energy generated by dielectric barrier discharge, so that the decomposition of the adhesive is facilitated, high-energy active particles in the generated plasma can interact with the adhesive, the decomposition of the adhesive is promoted, the time is saved, and the energy consumption is reduced; the dielectric barrier discharge binder removal increases the oxygen defect concentration in the ceramic green body, and has certain advantages in the aspects of subsequent surface regulation and sintering of the ceramic, namely, the voltage is lower in the subsequent ultrafast sintering process, and the ceramic green body is easier to sinter. The ultra-fast sintering method can realize the flash firing of the ceramic at room temperature, greatly reduce the environmental temperature required by the ceramic sintering and reduce a large amount of energy consumption; the ceramic sintering process is simple in flow, and compared with a common flash firing process, an additional heating device is not needed.
Drawings
Fig. 1 is a schematic structural view of an apparatus for a gas discharge-based ceramic green body processing method.
FIG. 2 is a schematic structural diagram of an apparatus for a room-temperature ultrafast ceramic sintering method;
FIG. 3 is a Fourier infrared spectrum of a ceramic green body without binder removal treatment and after 10min and 30min of binder removal treatment;
FIG. 4 is an Electron Paramagnetic Resonance (EPR) graph of a ceramic green body after binder removal and binder removal processing and a ceramic green body without binder removal processing in a conventional manner; DBD refers to a sample subjected to dielectric barrier discharge treatment; no DBD refers to a sample that has not been subjected to dielectric barrier discharge treatment;
description of reference numerals: 1-ceramic green body, 2-power supply, 3-electrode, 4-upper dielectric plate, 5-lower dielectric plate, 6-high voltage power supply, 7-fixed support and 8-lead.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1-2, a preferred embodiment of the present invention provides a room temperature ultra-fast sintering method of ceramic based on dielectric barrier discharge glue-discharging treatment, which comprises the following steps:
s1, preparing a ceramic green body 1, wherein the ceramic green body 1 contains a binder;
s2, vertically arranging two electrodes 3 in a plate-plate mode, enabling an upper dielectric plate 4 to be tightly attached to the upper electrode 3 and a lower dielectric plate 5 to be tightly attached to the lower electrode 3, placing a ceramic green body 1 in the center of the lower dielectric plate 5, adjusting the distance between the two electrodes 3, and connecting the two electrodes 3 with a power supply 2;
s3, setting the power supply frequency, increasing the voltage value to a target voltage peak value at a certain boosting rate, maintaining for a period of time after the discharge tends to be stable, and then reducing the voltage and cutting off the power supply 2 to finish the treatment process;
s4, spraying electrodes on two ends of the processed ceramic green body 1, winding the electrodes at the two ends by using a lead 8, and connecting the electrodes with a high-voltage power supply 6 through the lead 8;
and S5, switching on a high-voltage power supply 6, and adjusting the firing voltage and current to perform room-temperature ultrafast sintering of the ceramic.
In step S1, the adhesive includes polyvinyl alcohol and/or polyvinyl acetal Ding Quanzhi. The shape of the ceramic green sheet 1 includes a regular shape such as a cylinder, a rectangular parallelepiped, or a dog bone shape.
In the step S2, the distance between the upper medium plate 4 and the upper surface of the ceramic green body 1 is 1-5mm.
In step S3, the power frequency is 6-14kHz, the boosting rate is 1-4kV/S, the peak-to-peak value of the target voltage is 15-40kV, and the maintaining time is 5-60min.
In the step S4, the electrodes sprayed on the two ends of the ceramic green body 1 after the binder removal treatment are a method of spraying gold or coating conductive silver paste, and the wires 8 wound on the electrodes can be metal wires with higher melting points such as platinum wires. Specifically, the platinum wire has a high melting point and can resist high temperature, and is a preferred choice. When conditions permit, a metal wire having good conductivity such as a copper wire may be used instead, but the present invention is not limited thereto.
The step S5 specifically includes the following steps: and switching on the high-voltage power supply 6, increasing the amplitude of the voltage until the current flowing through the ceramic green body 1 is suddenly increased and the voltage at two ends of the ceramic green body 1 is suddenly reduced, and cutting off the power supply after a period of time is maintained to obtain the ceramic after the ultrafast sintering. Wherein the high-voltage power supply 6 is an alternating current power supplyOr a DC power supply, the boosting rate of the boosted voltage is 0.1-1kV/s, and the current density range is 10-150mA/mm 2 。
The following are specific examples.
The preparation of the green zinc oxide ceramic body mentioned in the following examples is as follows: selecting zinc oxide powder, adding 5% polyvinyl alcohol solution by mass according to 10% of the zinc oxide powder, and grinding until the zinc oxide powder passes through a 80-mesh screen for granulation. Weighing the granulated zinc oxide, pressing a wafer green compact with the thickness of 1mm and the diameter of 20mm under the pressure of 100MPa, and keeping the pressure for 5min to obtain the zinc oxide.
Example 1
The structure of the gas discharge-based ceramic green body glue discharging processing device is shown in figure 1, and the device comprises a power supply 2, two electrodes 3, an upper dielectric plate 4 and a lower dielectric plate 5. Wherein, the power supply 2 adopts a plasma high-frequency alternating current power supply CTP-2000K, the electrode 3 is a circular copper electrode, and the upper dielectric plate 4 and the lower dielectric plate 5 adopt high-temperature resistant insulating dielectric plates, such as 99 percent purity alumina ceramic dielectric plates. The specific connection mode is as follows: the two electrodes 3 are vertically arranged in a plate-plate mode, the upper dielectric plate 4 and the lower dielectric plate 5 are respectively attached to the upper electrode 3 and the lower electrode 3, and the ceramic green body 1 is placed in the middle of the upper surface of the lower dielectric plate 5. Two output terminals of the power supply 2 are respectively connected to the two electrodes 3, and a ground terminal of the power supply 2 is grounded. The boost rate is regulated by a voltage regulator.
The structure of the room temperature ultrafast sintering device provided by the invention is shown in fig. 2, the device comprises a high voltage power supply 6 and a fixed bracket 7, wherein: the both ends of pottery unburned bricks 1 are connected with high voltage power supply 6 through wire 8 respectively, and wire 8 is fixed and is made pottery unburned bricks 1 unsettled on fixed bolster 7. It is also possible to replace the fixing bracket 7 with an insulating ceramic plate, and to place the ceramic green sheet 1 on the insulating ceramic plate after connecting the lead wires 8 at both ends.
Example 2
The green zinc oxide ceramic compact 1 was subjected to a binder removal treatment and room temperature sintering using the apparatus in example 1. The ceramic green body 1 is in a dog bone shape, and the adhesive used for preparing the ceramic green body 1 can be polyvinyl alcohol and polyvinyl alcohol Ding Quanzhi.
And 2, turning on the power supply 2, setting the power supply frequency to be 12kHz, rotating a knob of a voltage regulator, boosting the voltage at the boosting rate of 3kV/s until the preset voltage peak value is 25kV, discharging tends to be uniform and stable after 1min, maintaining for 20min, reducing the voltage regulator to a zero position, and cutting off the power supply 2. The Electron Paramagnetic Resonance (EPR) behavior of the ceramic green body 1 after DBD treatment is shown in fig. 4.
And 3, carrying out a room-temperature ultra-fast sintering test on the zinc oxide ceramic green body 1 subjected to the binder removal treatment. And winding a lead 8 at two ends of the ceramic green body 1, connecting the lead 8 with the high-voltage power supply 6, and fixing the lead 8 on the bracket 7 to suspend the ceramic green body 1. The high-voltage power supply 6 adopts an alternating current power supply, the high-voltage power supply 6 is switched on, then the voltage is increased at the rate of 0.5kV/s, and the current density ranges from 10 mA/mm to 150mA/mm 2 And (3) until the voltage at the two ends of the ceramic green body 1 suddenly drops and the passing current suddenly rises, increasing the current to 600mA, and cutting off the power supply after maintaining for 1min to finish sintering. As a result, it was found that the initial firing voltage of the treated ceramic green sheet 1 after the ultrafast sintering at room temperature was 1.3kV, and no arc occurred during the sintering.
Comparative example 1
The zinc oxide ceramic green body 1 is directly subjected to the room temperature ultra-fast sintering test of the step 3 without the treatment of the steps 1 and 2, and the experimental parameters are the same as those of the example 1. The initial sintering voltage of the ceramic green body 1 which is not subjected to glue discharging treatment and subjected to ultra-fast sintering at room temperature is 2.6kV, and electric arcs appear in the sintering process, so that the surface of the ceramic is partially burnt by the electric arcs.
Comparing example 2 with comparative example 1, it was found that the room temperature sintering initiation voltage of the treated ceramic green body was reduced by half compared with that of the ceramic green body which was not subjected to binder removal treatment, and the problem that the arc and the like were difficult to control did not occur. The discharge treatment increases the oxygen defect concentration in the ceramic green body, and has certain advantages in the aspects of subsequent surface regulation and sintering of the ceramic and the like.
Fourier infrared spectra of the ceramic green body and the samples obtained in example 1 after 10min and 30min of dielectric barrier discharge treatment are shown in FIG. 3, and it can be seen that the wave numbers where the transmittance is obviously increased are 3200-3600cm -1 、1400-1600cm -1 、600-1000cm -1 This is consistent with the main peak position of the infrared spectrum of polyvinyl alcohol, which shows that the invention really realizes the decomposition and escape of the adhesive polyvinyl alcohol effectively.
Comparative example 2
The prepared zinc oxide ceramic green body is placed in a KSL-1750X muffle furnace for traditional binder removal, namely, the temperature is raised to 450 ℃ from room temperature at the heating rate of 2K/min, the temperature is kept for 2 hours, and then the temperature is naturally cooled to room temperature.
The Electron Paramagnetic Resonance (EPR) behavior of the ceramic green sheet 1 without binder removal, the conventional binder removal (comparative example 2), and the sample of example 1 are shown in fig. 4. By comparison, the sample after DBD ejection showed an increase in strength at g =1.96, which corresponds to Zn 2+ Nearby unpaired electrons, which means that the plasma action at atmospheric pressure causes an increase in oxygen defects in the sample. Compared with the traditional glue discharging mode, the glue discharging time is greatly shortened, namely the energy consumption of the ceramic green body in unit volume is reduced to below 10 percent of that of the traditional process.
In addition, the ceramic density and grain size of example 2 were measured, and it was found that the ceramic density was as high as 95%, defects such as cracks were not generated, and the average grain size was 0.8 μm and could be controlled to 1 μm or less.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.
Claims (10)
1. A room-temperature ultrafast sintering method of ceramic based on dielectric barrier discharge binder removal treatment is characterized by comprising the following steps:
s1, preparing a ceramic green body (1), wherein the ceramic green body (1) contains a binder;
s2, vertically oppositely arranging two electrodes (3) plate by plate, tightly attaching an upper dielectric plate (4) to the upper electrode (3) and tightly attaching a lower dielectric plate (5) to the lower electrode (3), placing the ceramic green body (1) in the center of the lower dielectric plate (5), adjusting the distance between the two electrodes (3), and connecting the two electrodes (3) with a power supply (2);
s3, setting power supply frequency, increasing the voltage value to a target voltage peak value at a certain boosting rate, maintaining for a period of time after the discharge tends to be stable, and then reducing the voltage and cutting off the power supply to finish the glue discharging process;
s4, spraying electrodes on two ends of the ceramic green body (1) subjected to the glue removing treatment, winding the electrodes at the two ends by using a lead (8), and connecting the electrodes with a high-voltage power supply (6) through the lead (8);
and S5, switching on a high-voltage power supply (6), and adjusting the firing voltage and current to perform room-temperature ultra-fast sintering of the ceramic.
2. The ultra-fast sintering method at room temperature for ceramic based on dielectric barrier discharge glue discharging treatment of claim 1, wherein the shape of the ceramic green body (1) in step S1 comprises a cylinder, a cuboid or a dog bone shape.
3. The method of claim 1, wherein in step S1, the binder comprises polyvinyl alcohol and/or polyvinyl acetal Ding Quanzhi.
4. The ultra-fast sintering method at room temperature for ceramics based on dielectric barrier discharge binder removal processing as claimed in claim 1, wherein in step S2, the distance between the upper dielectric plate (4) and the upper surface of the ceramic green body (1) is 1-5mm.
5. The method according to claim 1, wherein in step S3, the power frequency is 6-14kHz.
6. The method of claim 1, wherein in step S3, the step-up rate is 1 to 4kV/S, and/or the peak-to-peak target voltage is 15 to 40kV, and the holding time is 5 to 60min.
7. The ultra-fast sintering method at room temperature for ceramic based on dielectric barrier discharge gel discharge treatment of claim 1, wherein in step S4, the ceramic green body (1) is placed in the air or on an insulating ceramic plate.
8. The ultra-fast sintering method at room temperature for ceramic based on dielectric barrier discharge binder removal processing as claimed in claim 1, wherein in step S4, the method of spraying gold or coating conductive silver paste on the electrodes for spraying electrodes at two ends of the ceramic green body (1) after binder removal processing is adopted, and the lead (8) wound on the electrodes is made of platinum wire.
9. The method for ultrafast sintering of ceramic at room temperature based on dielectric barrier discharge binder removal processing as claimed in claim 1, wherein step S5 specifically comprises the steps of: and switching on the high-voltage power supply (6), increasing the amplitude of the voltage until the current flowing through the ceramic green body (1) is suddenly increased and the voltage at two ends of the ceramic green body (1) is suddenly reduced, and switching off the high-voltage power supply (6) after maintaining for a period of time to obtain the ceramic after ultrafast sintering.
10. The method for ultrafast sintering of ceramic at room temperature based on dielectric barrier discharge degumming treatment as claimed in claim 9, wherein the high voltage power supply (6) is an ac power supply or a dc power supply, the boosting rate of the boosted voltage is 0.1-1kV/s, and the current density ranges from 10 to 150mA/mm 2 。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110174333A1 (en) * | 2008-07-16 | 2011-07-21 | Agc Glass Europe | Process and installation for surface preparation by dielectric barrier discharge |
| CN110425877A (en) * | 2019-08-07 | 2019-11-08 | 清华大学深圳研究生院 | Ceramic post sintering device and ceramic post sintering method |
| 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 |
| CN113307624A (en) * | 2021-05-13 | 2021-08-27 | 佛山华骏特瓷科技有限公司 | Method for sintering ceramic at room temperature |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110174333A1 (en) * | 2008-07-16 | 2011-07-21 | Agc Glass Europe | Process and installation for surface preparation by dielectric barrier discharge |
| CN110425877A (en) * | 2019-08-07 | 2019-11-08 | 清华大学深圳研究生院 | Ceramic post sintering device and ceramic post sintering method |
| 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 |
| CN113307624A (en) * | 2021-05-13 | 2021-08-27 | 佛山华骏特瓷科技有限公司 | Method for sintering ceramic at room temperature |
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