CN115650736B - Ceramic room-temperature ultra-fast sintering method based on dielectric barrier discharge glue discharging treatment - Google Patents
Ceramic room-temperature ultra-fast sintering method based on dielectric barrier discharge glue discharging treatment Download PDFInfo
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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 glue discharging treatment, the ceramic green body has the advantages that the room-temperature sintering initial voltage is reduced by half, and the problem that electric arcs and the like are difficult to control is avoided. The invention realizes the room temperature ultrafast sintering of ceramics, realizes the great simplification of a sintering device and the great reduction of unit energy consumption rate, and compared with the traditional glue discharging device, the glue discharging device provided by the invention has the advantages of short time consumption and low energy consumption, can increase the oxygen defect of ceramic green bodies, has lower voltage in the subsequent ultrafast sintering process and is easier to enter sintering.
Description
Technical Field
The invention relates to the technical field of ceramic material preparation, in particular to a ceramic room-temperature ultra-fast sintering method based on dielectric barrier discharge glue discharging treatment.
Background
The ceramic material is a nonmetallic material with extremely wide application range, and can be used in the advanced fields of electronics, biomedical science, aerospace and other science and technology.
The glue discharging is a key link in the ceramic production process, has obvious influence on the performance of the formed ceramic, but the traditional heating glue discharging process has the defects of high time consumption, high energy consumption, high pollution and the like, so the design of the novel rapid and low-energy-consumption glue discharging process has important practical significance.
Ceramic materials are produced by requiring long times of high temperature to sinter an otherwise relatively loose green body to full densification. This means that the conventional ceramic manufacturing process requires a lot 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 press sintering, etc., have been proposed and put into practical use.
The flash firing technology is a novel electric field assisted sintering technology which appears in 2010, namely, the ceramic green body can be highly densified in a short period of seconds to minutes by applying proper alternating current or direct current voltage to two ends of the ceramic green body, and meanwhile, the furnace temperature required by ceramic sintering is greatly reduced. Such a short sintering time and relatively low furnace temperature means that the energy consumption required for the flash firing technique is greatly reduced compared to conventional sintering processes. However, overgrowth of ceramic grains often occurs during the firing process, and the grain size is too large, thereby affecting the service performance of the ceramic material. Therefore, the inhibition of grain growth in the process of flash burning has important significance for further popularization and application of the flash burning technology.
Disclosure of Invention
The invention aims to at least overcome one of the defects and shortcomings of the prior art and provides a ceramic room temperature ultra-fast sintering method based on dielectric barrier discharge glue discharging treatment. The invention is realized based on the following technical scheme:
the invention provides a ceramic room temperature ultra-fast sintering method based on dielectric barrier discharge glue discharge treatment, which comprises the following steps:
s1, preparing a ceramic green body, wherein the ceramic green body (1) contains a binder;
s2, vertically opposite two electrode plates, wherein an upper dielectric plate is closely attached to an upper electrode, a lower dielectric plate is closely attached to a lower electrode, a ceramic green compact is arranged at the center of the lower dielectric plate, the distance between the two electrodes is adjusted, and the two electrodes are connected with a power supply;
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 discharge tends to be stable, and then reducing the voltage to cut off the power supply to finish the glue discharging treatment process;
s4, spraying electrodes on two ends of the ceramic green body subjected to the glue discharging treatment, winding the ceramic green body at two ends by using wires, and connecting the ceramic green body with a high-voltage power supply through the wires;
s5, switching on a high-voltage power supply, and performing room-temperature ultrafast sintering of the ceramic by adjusting firing voltage and current.
Preferably, in step S1, the shape of the ceramic green body includes a cylindrical body, a rectangular parallelepiped, or a dog bone shape.
Preferably, in step S1, the binder comprises polyvinyl alcohol, and/or polyvinyl alcohol Ding Quanzhi.
Preferably, in step S2, the upper dielectric plate is spaced from the upper surface of the ceramic green body by a distance of 1-5mm.
Preferably, in step S3, the power supply frequency is 6-14kHz.
Preferably, the step-up rate in step S3 is 1-4kV/S.
Preferably, in step S3, the peak-to-peak value of the target voltage is 15-40kV, and the maintaining time is 5-60min.
Preferably, in step S4, the electrodes are sprayed on both ends of the treated ceramic green body by spraying metal or applying conductive silver paste, and the wire wound on the electrodes may be a metal wire with a higher melting point, such as a platinum wire.
Preferably, in step S4, the ceramic green body is suspended 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 suddenly increases, the voltage at two ends of the ceramic green body suddenly drops, and switching off the high-voltage power supply after a period of time to obtain the ceramic after ultra-fast 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 at least obtain one of the following beneficial effects:
the reactor is heated by heat energy generated by medium 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 can be saved, and the energy consumption can be reduced; the dielectric barrier discharge glue discharge 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 lower voltage and easier sintering in the subsequent ultra-fast sintering process. The ultra-fast sintering method can realize ceramic flash sintering at room temperature, greatly reduce the environmental temperature required by ceramic sintering and reduce a large amount of energy consumption; the ceramic sintering process is simple in flow and does not need an additional heating device compared with a common flash sintering process.
Drawings
FIG. 1 is a schematic view of an apparatus structure of a ceramic green body treatment method based on gas discharge.
FIG. 2 is a schematic diagram of the structure of a device for the ceramic room temperature ultra-fast sintering method;
FIG. 3 is a Fourier infrared spectrum of a ceramic green body without glue removal treatment, after 10min and 30min of glue removal treatment;
FIG. 4 is an Electron Paramagnetic Resonance (EPR) diagram of a ceramic green body after the adhesive discharging treatment and a ceramic green body without the adhesive discharging treatment in a conventional manner; DBD refers to a sample subjected to dielectric barrier discharge treatment; no DBD refers to a sample not subjected to dielectric barrier discharge treatment;
reference numerals illustrate: the ceramic green body comprises a 1-ceramic green body, a 2-power supply, a 3-electrode, a 4-upper dielectric plate, a 5-lower dielectric plate, a 6-high voltage power supply, a 7-fixed support and an 8-wire.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
As shown in fig. 1-2, the preferred embodiment of the invention provides a ceramic room temperature ultra-fast sintering method based on dielectric barrier discharge glue discharge treatment, which comprises 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 in a plate-plate mode, wherein an upper dielectric plate 4 is clung to the upper electrode 3, a lower dielectric plate 5 is clung to the lower electrode 3, a ceramic green body 1 is arranged at the center of the lower dielectric plate 5, the distance between the two electrodes 3 is adjusted, and the two electrodes 3 are connected 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 to cut off the power supply 2 to finish the treatment process;
s4, spraying electrodes on two ends of the treated ceramic green body 1, winding the treated ceramic green body with wires 8 at two ends, and connecting the treated ceramic green body with a high-voltage power supply 6 through the wires 8;
s5, switching on the high-voltage power supply 6, and performing room-temperature ultrafast sintering of the ceramic by adjusting firing voltage and current.
In step S1, the adhesive includes polyvinyl alcohol, and/or polyvinyl alcohol Ding Quanzhi. The shape of the ceramic green body 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 dielectric plate 4 and the upper surface of the ceramic green body 1 is 1-5mm.
In the step S3, the power supply frequency is 6-14kHz, the boosting rate is 1-4kV/S, the peak value of the target voltage peak is 15-40kV, and the maintaining time is 5-60min.
In step S4, the electrodes are sprayed on the two ends of the ceramic green body 1 after the glue discharging treatment by adopting a method of spraying metal 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 higher melting point, can withstand high temperature, and is a preferred choice. If the conditions allow, a wire having good conductivity such as a copper wire may be used instead of the wire, and the wire is not limited to this.
The step S5 specifically comprises 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 suddenly increases, the voltage at the two ends of the ceramic green body 1 suddenly drops, and cutting off the power supply after a period of time to obtain the ceramic after ultra-fast sintering. Wherein the high-voltage power supply 6 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 following are specific examples.
The preparation method of the zinc oxide ceramic green body mentioned in the following examples is as follows: zinc oxide powder is selected, polyvinyl alcohol solution with the mass fraction of 5% is added according to the mass percentage of 10%, and grinding is carried out until the granules are granulated through a 80-mesh screen. Weighing the granulated zinc oxide, and pressing a wafer green body with the thickness of 1mm and the diameter of 20mm at the pressure of 100MPa for 5min to obtain the zinc oxide.
Example 1
The structure of the ceramic green body glue discharging treatment device based on gas discharge 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% purity alumina ceramic dielectric plates. The specific connection mode is as follows: the two electrodes 3 are vertically opposite, an upper dielectric plate 4 and a lower dielectric plate 5 are respectively closely attached to the upper electrode 3 and the lower electrode 3, and a ceramic green body 1 is placed on the upper surface of the lower dielectric plate 5 in a centering manner. The two output ends of the power supply 2 are respectively connected to the two electrodes 3, and the grounding end of the power supply 2 is grounded. The boost rate is regulated by a voltage regulator.
The structure of the room temperature ultra-fast sintering device provided by the invention is shown in fig. 2, and the device comprises a high-voltage power supply 6 and a fixed bracket 7, wherein: the two ends of the ceramic green body 1 are respectively connected with the high-voltage power supply 6 through leads 8, and the leads 8 are fixed on a fixed support 7 so that the ceramic green body 1 can be suspended. The fixing support 7 can also be replaced by an insulating ceramic plate, and the ceramic green body 1 is placed on the insulating ceramic plate after the two ends are connected with the wires 8.
Example 2
The zinc oxide ceramic green body 1 was subjected to a paste ejection treatment and room temperature sintering using the apparatus of example 1. The ceramic green body 1 is dog bone-shaped, and the adhesive used for preparing the ceramic green body 1 can be polyvinyl alcohol or polyvinyl acetal 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 by 3kV/s to a preset voltage peak value of 25kV, enabling discharge to be uniform and stable after 1min, maintaining for 20min, enabling the voltage regulator to be reduced to a zero position, and cutting off the power supply 2. The Electron Paramagnetic Resonance (EPR) situation of the ceramic green body 1 after DBD treatment is shown in fig. 4.
And 3, performing a room-temperature ultra-fast sintering test on the zinc oxide ceramic green body 1 subjected to the glue discharging treatment. The two ends of the ceramic green body 1 are wound with the lead wires 8, the lead wires 8 are connected with the high-voltage power supply 6, and the lead wires 8 are fixed on the support 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 connected, then the voltage is increased at the speed of 0.5kV/s, and the current density is in the range of 10-150mA/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 after maintaining for 1min, switching off the power supply to finish sintering. As a result, it was found that the initial firing voltage of the room temperature ultrafast sintering of the treated ceramic green body 1 was 1.3kV, and no arc occurred during the sintering.
Comparative example 1
The zinc oxide ceramic green body 1 was directly subjected to the room temperature ultrafast sintering test of step 3, the treatments of steps 1 and 2 were not performed, and experimental parameters were the same as in example 1. The initial sintering voltage of the ceramic green body 1 which is not subjected to glue discharge treatment and is subjected to ultra-fast sintering at room temperature is 2.6kV, and an arc appears in the sintering process, so that part of the surface of the ceramic is burnt by the arc.
Comparison of example 2 and comparative example 1 shows that the room temperature sintering initiation voltage of the treated ceramic green body is reduced by half compared with that of the ceramic green body without the paste discharging treatment, and the problem of difficult control such as arc and the like does 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.
Fourier infrared spectra of the ceramic green body and samples obtained after 10min and 30min of dielectric barrier discharge treatment in example 1 are shown in FIG. 3, and the wave numbers at the positions with obviously increased transmittance are 3200-3600cm respectively -1 、1400-1600cm -1 、600-1000cm -1 This coincides with the main peak position of the infrared spectrum of the polyvinyl alcohol, which shows that the invention really and effectively realizes the decomposition and escape of the adhesive polyvinyl alcohol.
Comparative example 2
The prepared zinc oxide ceramic green body is placed in a KSL-1750X muffle furnace for traditional glue discharging, namely, the temperature is raised to 450 ℃ from the room temperature at the heating rate of 2K/min, the heat is preserved for 2 hours, and then the natural heat is radiated to the room temperature.
The Electron Paramagnetic Resonance (EPR) of the ceramic green body 1, the conventional paste (comparative example 2), and the sample of example 1, which were not subjected to paste discharge treatment, are shown in fig. 4. Comparison found that the sample increased in strength at g=1.96 after DBD gum removal, 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 per unit volume is reduced to below 10% of that of the traditional process.
In addition, the ceramic density and particle size of example 2 were examined, 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, which could be controlled to 1 μm or less.
Finally, it should be noted that: the foregoing description of the preferred embodiments of the present invention is not intended to be limiting, but rather, it will be apparent to those skilled in the art that the foregoing description of the preferred embodiments of the present invention can be modified or equivalents can be substituted for some of the features thereof, and any modification, equivalent substitution, improvement or the like that is within the spirit and principles of the present invention should be included in the scope of the present invention.
Claims (6)
1. The ceramic room temperature ultra-fast sintering method based on dielectric barrier discharge glue discharge treatment is characterized by comprising the following steps of:
s1, preparing a ceramic green body (1), wherein the ceramic green body (1) contains a binder;
s2, vertically opposite two electrode plates, wherein an upper dielectric plate (4) is clung to an upper electrode, a lower dielectric plate (5) is clung to a lower electrode, a ceramic green body (1) is arranged at the center of the lower dielectric plate (5), the distance between the two electrodes is adjusted, and the two electrodes are connected 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 discharge tends to be stable, and then reducing the voltage to cut off the power supply to finish the glue discharging treatment process;
s4, spraying electrodes on two ends of the ceramic green body (1) subjected to glue discharge treatment, winding the ceramic green body at two ends by using a wire (8), and connecting the ceramic green body with a high-voltage power supply (6) through the wire (8);
s5, switching on a high-voltage power supply (6), and performing room-temperature ultrafast sintering of the ceramic by adjusting firing voltage and current;
in step S1, the binder comprises polyvinyl alcohol, and/or polyvinyl alcohol Ding Quanzhi;
in the step S2, the distance between the upper dielectric plate (4) and the upper surface of the ceramic green body (1) is 1-5mm;
in the step S3, the power supply frequency is 6-14kHz; in the step S3, the boosting rate is 1-4kV/S, the peak value of the target voltage peak is 15-40kV, and the maintaining time is 5-60min.
2. The method for ultra-fast sintering ceramic at room temperature based on dielectric barrier discharge paste ejection treatment according to claim 1, wherein the shape of the ceramic green body (1) in step S1 comprises a cylindrical, rectangular or dog bone shape.
3. The method for ultra-fast sintering at room temperature of ceramic based on dielectric barrier discharge glue discharge treatment according to claim 1, wherein in step S4, the ceramic green body (1) after the glue discharge treatment is placed in suspension or on an insulating ceramic plate.
4. The method for ultra-fast sintering of ceramic room temperature based on dielectric barrier discharge glue discharge treatment according to claim 1, wherein in step S4, electrodes are sprayed on two ends of the ceramic green body (1) after the glue discharge treatment by adopting a method of metal spraying or conductive silver paste coating, and wires (8) wound on the electrodes adopt platinum wires.
5. The method for ultra-fast sintering ceramic at room temperature based on dielectric barrier discharge glue discharge treatment according to claim 1, wherein the step S5 specifically comprises 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) after the glue discharging treatment suddenly increases, the voltage at two ends of the ceramic green body (1) after the glue discharging treatment suddenly drops, and switching off the high-voltage power supply (6) after a period of time is maintained, so as to obtain the ceramic after ultra-fast sintering.
6. The method for ultra-fast sintering ceramic room temperature based on dielectric barrier discharge paste discharge treatment according to claim 5, wherein the high-voltage power supply (6) is an alternating current power supply or a direct current power supply, the boosting rate of the boosting voltage is 0.1-1kV/s, and the current density range is 10-150mA/mm 2 。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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| EP2145701A1 (en) * | 2008-07-16 | 2010-01-20 | AGC Flat Glass Europe SA | Method and installation for surface preparation by dielectric barrier discharge |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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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