CN110606751B - Method for graphene-assisted room-temperature flash firing of ceramic material - Google Patents
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Abstract
The invention relates to a method for graphene-assisted room-temperature flash firing of a ceramic material, which comprises the steps of dispersing graphene into a solvent, and mixing to obtain a graphene solution; adding ceramic powder into the graphene solution, uniformly mixing, and removing the solvent to obtain composite powder; the composite powder is formed into a blank body, and an electric field is applied to two ends of the blank body at room temperature, so that flash burning can be finished within a time of less than 60s at the fastest speed. Compared with the prior art, the method can generate flash firing under the condition of room temperature, the temperature of the ceramic blank body is rapidly increased to the initial temperature of the flash firing by using the Joule heat generated by electrifying, the blank body is rapidly shrunk by the flash firing, and the sintering is completed in a short time.
Description
Technical Field
The invention relates to a method for manufacturing a ceramic material, in particular to a method for graphene-assisted room-temperature flash firing of the ceramic material.
Background
Flash sintering (Flash sintering) is to apply an electric field (7.5-1000V/cm) and a temperature field (the temperature of a furnace rises at a certain speed) to a ceramic blank, when the temperature of the furnace reaches a certain value (lower than the sintering temperature, the temperature is the initiation temperature of Flash sintering, and is called as 'Flash sintering temperature' for short), sintering occurs, and the energy density rises rapidly to reach an extreme value (can reach 10-1000 mW/mm)3). The process is accompanied by a non-linear increase in the conductivity of the sample, requiring less than 1 minute from flash-off to complete sintering. [ Raj et al.in a patent No. US 9,334,194 (2011)]Compared with the traditional sintering method, the method can complete the sintering at lower temperature in extremely short time. The sintered sample often has the characteristic of fine grains. Flash firing was initially only applicable to ion conductor ceramic materials with NTC effect (resistance decrease with temperature rise) and later developed toInsulator (Al)2O3) Semiconductor (SiC), and metal conductor (aluminum alloy). Although flash firing temperatures are already low compared to conventional sintering, there has been much research into how to reduce flash firing initiation temperatures, even when flash firing occurs at room temperature (room temperature sintering can reduce costs and save energy, simplifying sintering equipment-directly removing the equipment necessary for conventional sintering, i.e., the furnace). For example, the zinc oxide is flashed by introducing water vapor-containing hydrogen gas into a tube furnace at room temperature (Jiuyuan Nie, et al. Water-associated flash sintering: flash ZnO at room temperature to acetic acid-98% dense in seconds J)].Scripta Materialia,142(2018)79-82.]Room temperature flash-fired aluminum alloys [ Brandon McWilliams, et al].J Mater Sci,(2018)53:9297–9304]. In the first method, the requirements on equipment are not reduced, and the sintering temperature of the zinc oxide is not high; the second method, sintering is a metal material, which has high conductivity, and is not suitable for most inorganic non-metal materials with relatively low conductivity. Therefore, the above method is not universal, and a method of flash firing at room temperature which is simple and effective for most ceramic materials is sought.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for graphene-assisted room temperature flash firing of a ceramic material.
The purpose of the invention can be realized by the following technical scheme:
a method for flash-firing a ceramic material at room temperature by graphene assistance is characterized in that a high electric field is applied to two ends of a graphene reinforced ceramic composite material to limit relatively low current, and flash firing is performed at room temperature by utilizing the characteristic of high conductivity of graphene. The method comprises the following steps of providing flash firing initiation temperature by utilizing the temperature generated by graphene, conducting a blank, rapidly increasing the temperature of a ceramic blank to a sintering temperature by utilizing joule heat generated by electrifying, rapidly shrinking the blank, and completing sintering in a short time (1min), wherein the method comprises the following steps:
dispersing graphene into a solvent, and mixing to obtain a graphene solution;
adding ceramic powder into the graphene solution, uniformly mixing, and removing the solvent to obtain composite powder;
and (3) forming the composite powder into a blank, applying an electric field to two ends of the blank at room temperature, and finishing flash firing within the time of less than 60 s.
Further, the electric field intensity is 20-1000V/cm; furthermore, the electric field strength is 20-1000V/cm.
Further, the current density is 40-500 mA/mm2(ii) a Furthermore, the current density is 40 to 500mA/mm2。
Further, after the electric field is applied for electrifying, the increasing speed of the current is controlled to be less than 1mA/s, the slowly increasing time is called a 'incubation period', the time is related to the field intensity and lasts for 1-30 s, the current in the middle period rapidly increases at the speed of 10-1000 mA/s and lasts for 1-10s, and finally the current reaches the maximum value and enters a stabilization period to keep the material sintered and compact for 5-20 s.
Further, the graphene is graphene nanoplatelets, graphene oxide or reduced graphene oxide, and the solvent is deionized water, ethanol, DMF or NMP.
Further, the concentration of the graphene solution is 0.02-8 mg/mL.
Further, the ceramic powder is YSZ, a semiconductor or an insulator.
Still further, the semiconductor comprises silicon carbide and the insulator comprises alumina.
Further, the ceramic powder is ball-milled in the graphene solution and uniformly mixed, and the solvent is removed in an oven.
Further, the content of graphene in the composite powder is 1-10 wt%.
Further, the blank is in the shape of a dog bone, a strip, a cylinder or a disc, an electric field is applied to two ends of the pressed blank, and the length of the blank in the direction of the electric field is 1-50 cm.
Compared with the prior art, the invention has the following advantages:
(1) the room temperature flash burning is fast, and the heating time of the furnace and the energy consumed in the period are saved. The traditional method for sintering ceramics is to radiate heat to a green body through a furnace, which requires tens of minutes or even hours, and the efficiency is far lower than the heating mode of directly flash-burning the green body to generate joule heat, so that flash-burning only needs a few minutes to sinter the green body.
(2) The room temperature sintering can reduce the cost and save energy, and more importantly, can greatly simplify the sintering equipment and save the equipment which is necessary for a furnace regardless of the traditional sintering process and the flash firing process. The blank needs to be heated by a furnace to provide certain heat to enable the blank to reach the initiation temperature of flash combustion, and the heat generated by electrifying uniformly dispersed graphene in the blank replaces the heat of the furnace.
(3) The addition amount of the graphene filler in the method is low, and compared with other conductive fillers needing to be added in a large amount, the graphene filler does not have great adverse effect on sintering. This is related to the characteristics of graphene, which is a material with an ultra-large specific surface area and high conductivity.
Drawings
FIG. 1 is a photograph of a product obtained in example 1;
FIG. 2 is a graph showing the change of field intensity and current density with time in example 1;
FIG. 3 is a graph of energy density and sample shrinkage over time for example 1.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
A method for graphene-assisted room-temperature flash firing of a ceramic material comprises the following steps:
(1) weighing a certain amount of graphene (graphene nanoplatelets, graphene oxide or reduced graphene oxide), dispersing in a proper solvent (deionized water, ethanol, DMF or NMP), stirring for 20-180min to obtain a uniform graphene solution, and controlling the concentration of the graphene solution to be 0.02-8 mg/mL;
(2) adding a certain amount of ceramic powder (ionic conductor such as YSZ, semiconductor such as silicon carbide, insulator such as aluminum oxide) into the prepared graphene solution, uniformly mixing by a ball milling method, wherein the ball milling speed is 100-1000r/min, the ball milling time is 2-24h, and removing the solvent in an oven to obtain composite powder (the final graphene content is 1-10 wt%);
(3) adding a proper amount of prepared composite powder into a mold, pressing into a dog bone shape, a strip shape, a cylinder shape or a disc shape, and applying an electric field to two ends of a pressed blank body, wherein the length of the blank body in the direction of the electric field is 1-50 cm;
(4) under the condition of room temperature, the electric field intensity required by sintering the green body is required to be more than 20V/cm, and the current density is more than 40mA/mm2After the ceramic material is electrified, the current is slowly increased and then rapidly increased, the current reaches the maximum value finally, the sintering of the ceramic material is realized, and the time of the whole process is less than 60 s.
The following are more detailed embodiments, and the technical solutions and the technical effects obtained by the present invention will be further described by the following embodiments.
The ball mill used in each example was a planetary ball mill manufactured by Nanda instruments Inc. of Nanjing. The electric heating air-blast drying box is a DHG9040HA type electric heating air-blast drying box produced by Zhejiang Hangzhou blue sky laboratory. The tablet press is manufactured by mixcrystal company. The power supply is produced by Dinghua corporation with the range of voltage 0-1000V and current 0-1A.
Example 1:
a method for graphene-assisted room-temperature flash firing of a ceramic material comprises the following steps:
(1) weighing a certain amount of graphene oxide produced by Shanghai carbon source Huogu new material science and technology Limited, dispersing in deionized water, and stirring for 60min to obtain a uniform graphene oxide solution, wherein the concentration of the solution is 2 mg/mL;
(2) adding a certain amount of YSZ (yttrium stabilized zirconia) powder into the prepared graphene oxide solution, uniformly mixing by using a planetary ball milling method, wherein the ball milling speed is 300r/min, the ball milling time is 12h, removing the solvent in an oven to obtain composite powder of YSZ and graphene oxide, and finally, the content of the graphene oxide is 2 wt%;
(3) 0.8g of the prepared composite powder is added into a mould and pressed into a dog bone shape as shown in figure 1. The size of the blank is 20X 3X 2mm3Platinum wire is used to apply field strength through holes at both ends. Applying an electric field to two ends of the pressed green body, wherein the length of the green body in the direction of the electric field is 20 mm;
(4) under the condition of room temperature, the electric field intensity required by sintering the green body is 60V/cm, and the current density is 160mA/mm2After the electric field is applied for electrifying, the increasing speed of the current is controlled to be less than 1mA/s, the current is slowly increased for 30s, the current in the middle period is rapidly increased at the speed of 10mA/s for 10s, the current finally reaches the maximum value and enters the stable period, the sintering compactness of the material for 20s is kept, the sintering of the ceramic material is realized, and the time for the whole process is 60 s.
Example 2:
a method for graphene-assisted room-temperature flash firing of a ceramic material comprises the following steps:
(1) weighing a certain amount of graphene nanoplatelets, dispersing the graphene nanoplatelets in ethanol, and stirring for 120min to obtain a uniform graphene solution, wherein the concentration of the solution is 4 mg/mL;
(2) adding a certain amount of alumina powder into the prepared graphene solution, uniformly mixing by using a planetary ball milling method, wherein the ball milling speed is 300r/min, the ball milling time is 12h, removing the solvent in an oven to obtain composite powder of alumina and graphene, and finally, the graphene content is 5 wt%;
(3) adding 0.8g of the prepared composite powder into a mold, and pressing into dog bone shape, wherein the size of the blank body is 20 multiplied by 3 multiplied by 2mm3Applying an electric field to two ends of the pressed green body, wherein the length of the green body in the direction of the electric field is 30 mm;
(4) under the condition of room temperature, the electric field intensity required by sintering the green body is 70V/cm, and the current density is 100mA/mm2After applying electric field, the initial current is less than 1mA/sThe speed of the ceramic material is slowly increased for 10s, the current in the middle period is rapidly increased at the speed of 1000mA/s for 10s, the current reaches the maximum value finally and enters the stable period, the sintering compactness of the 10s material is kept, the sintering of the ceramic material is realized, and the time of the whole process is 30 s.
Example 3:
a method for graphene-assisted room-temperature flash firing of a ceramic material comprises the following steps:
(1) weighing a certain amount of reduced graphene oxide reduced by ascorbic acid, dispersing in ethanol, and stirring for 60min to obtain a uniform reduced graphene oxide solution, wherein the concentration of the solution is 4 mg/mL;
(2) adding a certain amount of silicon carbide powder into the prepared reduced graphene oxide solution, uniformly mixing by using a planetary ball milling method, wherein the ball milling speed is 300r/min, the ball milling time is 12 hours, removing the solvent in an oven to obtain composite powder of silicon carbide and reduced graphene oxide, and finally, the content of the reduced graphene oxide is 2 wt%;
(3) adding 0.8g of the prepared composite powder into a mold, and pressing into dog bone shape, wherein the size of the blank body is 20 multiplied by 3 multiplied by 2mm3Applying an electric field to two ends of the pressed green body, wherein the length of the green body in the direction of the electric field is 20 mm;
(4) under the condition of room temperature, the electric field intensity required by sintering the green body is 100V/cm, and the current density is 160mA/mm2After the electric field is applied for electrifying, the initial current is slowly increased at the speed of less than 1mA/s for 5s, the middle current is rapidly increased at the speed of 800mA/s for 10s, the final current reaches the maximum value and enters a stable period, the 5s material sintering compactness is kept, the sintering of the ceramic material is realized, and the time of the whole process is 20 s.
Fig. 2 and 3 are graphs of field strength, current density, energy density, and sample shrinkage over time in accordance with the present invention. As can be seen from the figure, the present invention applies a high field strength (60V/cm), and the current starts to increase slowly and then rises rapidly to reach the preset value (160 mA/mm)2) The sample began to shrink at this point, shrinking 25% over 20 seconds, completing the sintering.
Example 4
A method for graphene-assisted room-temperature flash firing of a ceramic material comprises the following steps:
(1) weighing a certain amount of graphene nanoplatelets, dispersing the graphene nanoplatelets in deionized water, and stirring for 20min to obtain a uniform graphene solution, wherein the concentration of the solution is 0.02 mg/mL;
(2) adding a certain amount of YSZ powder into the prepared graphene solution, uniformly mixing by using a planetary ball milling method, wherein the ball milling speed is 100r/min, carrying out ball milling for 2h, removing the solvent in an oven to obtain composite powder of YSZ and graphene, and finally, the graphene content is 1 wt%;
(3) adding 0.8g of prepared composite powder into a mould, pressing into a strip shape, wherein the size of a blank body is 20 multiplied by 3 multiplied by 2mm3Applying an electric field to two ends of the pressed green body, wherein the length of the green body in the direction of the electric field is 20 mm;
(4) under the condition of room temperature, the electric field intensity required by sintering the green body is 80V/cm, and the current density is 100mA/mm2After the electric field is applied for electrifying, the initial current is slowly increased at the speed of less than 1mA/s for 1s, the middle current is rapidly increased at the speed of 500mA/s for 5s, the final current reaches the maximum value and enters a stable period, the sintering compactness of the 14s material is kept, and the sintering of the ceramic material is realized, wherein the time is 30s in the whole process.
Example 5
A method for graphene-assisted room-temperature flash firing of a ceramic material comprises the following steps:
(1) weighing a certain amount of graphene oxide, dispersing the graphene oxide in ethanol, and stirring for 180min to obtain a uniform graphene oxide solution, wherein the concentration of the solution is 8 mg/mL;
(2) adding a certain amount of alumina powder into the prepared graphene oxide solution, uniformly mixing by using a planetary ball milling method, wherein the ball milling speed is 1000r/min, the ball milling time is 24 hours, removing the solvent in an oven to obtain composite powder of alumina and graphene oxide, and finally, the content of the graphene oxide is 10 wt%;
(3) adding 0.8g of prepared composite powder into a mold, pressing into a cylinder shape, and applying an electric field to two ends of a pressed blank body, wherein the length of the blank body in the direction of the electric field is 20 mm;
(4) under the condition of room temperature, the electric field intensity required by sintering the green body is 200V/cm, and the current density is 100mA/mm2After the electric field is applied for electrifying, the initial current is slowly increased at the speed of less than 1mA/s for 30s, the middle current is rapidly increased at the speed of 1000mA/s for 5s, the final current reaches the maximum value and enters a stable period, the sintering compactness of the material for 15s is kept, and the sintering of the ceramic material is realized, wherein the time for the whole process is 50 s.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean 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 invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. A method for graphene-assisted room temperature flash firing of a ceramic material is characterized by comprising the following steps:
dispersing graphene into a solvent, and mixing to obtain a graphene solution;
adding ceramic powder into the graphene solution, uniformly mixing, and removing the solvent to obtain composite powder; the content of graphene in the composite powder is 1-10 wt%;
forming the composite powder into a blank, and applying an electric field to two ends of the blank at room temperature;
after the electric field is applied for electrifying, the initial current is slowly increased at a speed of less than 1mA/s for 1-30 s, the middle current is rapidly increased at a speed of 10-1000 mA/s for 1-10s, the final current reaches the maximum value and enters a stable period, the material sintering compactness is kept for 5-20 s, the flash combustion is completed, the flash combustion speed is high, and the temperature rise time and the energy consumed during the period are saved.
2. The method of claim 1, wherein the electric field strength required for sintering the green body is greater than 20V/cm.
3. The method of claim 1, wherein the current density required for sintering the green body is greater than 40mA/mm2。
4. The method for graphene-assisted room temperature flash firing of a ceramic material according to any one of claims 1 to 3, wherein the graphene is graphene nanoplatelets, graphene oxide or reduced graphene oxide, and the solvent is deionized water, ethanol, DMF or NMP.
5. The method for room-temperature graphene-assisted flash firing of a ceramic material according to any one of claims 1 to 3, wherein the concentration of the graphene solution is 0.02-8 mg/mL.
6. The method for graphene-assisted room temperature flash firing of a ceramic material according to any one of claims 1 to 3, wherein the ceramic powder is YSZ, a semiconductor or an insulator, the semiconductor comprises silicon carbide, the insulator comprises alumina, the ceramic powder is ball-milled in a graphene solution and mixed uniformly, and the solvent is removed in an oven.
7. The method for graphene-assisted room temperature flash firing of a ceramic material according to any one of claims 1 to 3, wherein the shape of the green body is dog-bone shape, long strip shape, cylindrical shape or disc shape, an electric field is applied to two ends of the pressed green body, and the length of the green body in the direction of the electric field is 1-50 cm.
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| CN111535011A (en) * | 2020-06-08 | 2020-08-14 | 北京石墨烯研究院 | Method for preparing graphene fibers through joule heat flash evaporation |
| CN112024892B (en) * | 2020-08-27 | 2022-08-19 | 湖南艾华集团股份有限公司 | Method for manufacturing aluminum electrolytic capacitor anode foil by electric field auxiliary sintering |
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