CN112390629B - Device and method for rapidly sintering ceramic - Google Patents

Device and method for rapidly sintering ceramic Download PDF

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CN112390629B
CN112390629B CN202011398857.5A CN202011398857A CN112390629B CN 112390629 B CN112390629 B CN 112390629B CN 202011398857 A CN202011398857 A CN 202011398857A CN 112390629 B CN112390629 B CN 112390629B
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stainless steel
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CN112390629A (en
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沈平
郭瑞芬
毛海荣
赵志陶
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Jilin University
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Abstract

本发明涉及一种快速烧结陶瓷装置及方法，包括炉体、开设在炉体一侧的观察窗以及设置在炉体内的加压组件和测温组件，还包括通电组件与绝缘组件，炉体内腔中心处设有石墨模具，石墨模具内设有呈S形设置并放置有带有样品的石墨软毡，通电组件设置在石墨软毡上下方并与BN侧板相配合；快速烧结陶瓷方法包括以下步骤：压制、通电、升温、断电和降温；与传统烧结方法相比，该方法无需对炉体进行加热，加热速度快，烧结温度高，周期短，极大提高了生产效率，降低了能耗，同时丰富了陶瓷烧结技术，而且获得的陶瓷致密化程度更高，适用性更宽泛。

Figure 202011398857

The invention relates to a rapid sintering ceramic device and method, comprising a furnace body, an observation window opened on one side of the furnace body, a pressurizing component and a temperature measuring component arranged in the furnace body, and also includes an electrification component and an insulating component, and a furnace body cavity There is a graphite mold in the center, and a graphite soft felt with a sample is arranged in the graphite mold and placed in an S shape. The electrification components are arranged on the upper and lower parts of the graphite soft felt and cooperate with the BN side plates; the rapid sintering ceramic method includes the following Steps: pressing, energizing, heating, powering off and cooling; compared with the traditional sintering method, this method does not need to heat the furnace body, the heating speed is fast, the sintering temperature is high, and the cycle is short, which greatly improves the production efficiency and reduces the energy consumption. At the same time, the ceramic sintering technology is enriched, and the obtained ceramic has a higher degree of densification and wider applicability.

Figure 202011398857

Description

Device and method for rapidly sintering ceramic
Technical Field
The invention relates to the technical field of ceramic material processing, in particular to a device and a method for rapidly sintering ceramic.
Background
Ceramic materials are widely used in structural and functional fields due to their excellent properties such as high melting point, high strength, high hardness, and high temperature thermal stability. At present, the preparation technology of ceramic materials mainly comprises traditional high-temperature sintering, reaction sintering, hot isostatic pressing sintering and the like, the technologies usually rely on a thermal convection or a thermal radiation mode to heat ceramic green bodies, and the heating rate is low, the sintering period is long, and the energy utilization rate is low. For high temperature volatile ceramics (such as lithium ion battery materials), longer sintering times result in volatilization of components, thereby impairing the performance of the material.
In order to reduce the Sintering energy consumption and shorten the cycle time, Spark Plasma Sintering (SPS) has been proposed. The Chinese patent application number is 201110287859.1, and the inventor proposes a high-pressure sintering combined die and a high-pressure rapid sintering method for preparing nano ceramic by the same to Liugui Wu et al. They put the combined high-pressure sintering die filled with the nano ceramic powder into a plasma sintering furnace for sintering. Sintering the ceramic under the conditions that the heating rate is 100-300 ℃/min, the sintering pressure is 100-1000 MPa, the sintering temperature is 500-800 ℃, and the sintering heat preservation time is 3-10 min. When the conductive sample is sintered, current directly flows through the sample, and joule heat generated by the sample is used for realizing ceramic sintering. While the conductive samples are generally less resistive, which requires a larger (hundreds to thousands of amperes) dc pulse current. When sintering a non-conductive sample, current flows through the graphite mold, and the larger graphite mold heats the sample again by generating joule heat, which undoubtedly greatly reduces the heat utilization efficiency. The Chinese patent application No. 201910233609.6, the inventor proposes a metal oxide ceramic material fast sintering furnace and a sintering process thereof for Hexiangheng et al. The hearth is sequentially provided with a high-temperature chamber, a medium-temperature chamber and a low-temperature chamber which are communicated with each other from top to bottom. During sintering, the green body is sequentially fed into low-temperature, medium-temperature and high-temperature chambers to realize rapid sintering. This technique still requires preheating the chamber. This way of relying on furnace heating to achieve sample heating is inefficient because the rate of furnace heating is slow and the maximum temperature that can be achieved is relatively low (1700 c for a high temperature chamber). In 2010, the university of Colorado Raj invented a new technology, in which a Ceramic green compact with an initial density of 50% was sintered to be dense within 5s at a field strength of 120V/cm and a temperature of 850 ℃, and this technology was called Flash Sintering because of the Flash phenomenon during Sintering (Flash Sintering of Nanograin Zirconia in <5s at 850 ℃, Journal of the American Ceramic Society, Vol. 93 in 2010, No. 11, P3556-P3559). The inventor of Chinese patent application No. 201910058819.6 proposes a method for rapidly sintering NBT piezoelectric ceramics at low temperature by Pu Yong Ping et al, which belongs to the flash firing technology. In the flash burning process, the sample is connected with two ends of a power supply through electrodes, and the sintering is realized by using joule heat generated when current flows through the sample. This requires that the sample have some electrical conductivity. However, most of the ceramic materials are not conductive or have weak conductivity at room temperature, and the ceramic materials need to be heated to a higher temperature to have certain ionic or electronic conductivity. Therefore, in flash firing, it is usually necessary to heat the furnace body to a certain temperature (typically several hundred degrees) to make the sample have a certain conductivity. Furthermore, the greatest disadvantage of flash firing technology is that the sample sintering is not uniform, and the critical conditions under which flash firing occurs are largely dependent on the power supply capability (e.g., extremely high voltages are required to drive the movement of ions or electrons within the ceramic material), which results in a large compromise in its universality and economy. The flash firing technology is only suitable for single-piece production, special requirements are placed on samples, and meanwhile, the traditional electric kiln has the defects of long sintering period, high energy consumption, low energy utilization rate and high cost when being used for preparing ceramic materials, is poor in adaptability and needs to be improved.
Disclosure of Invention
In order to achieve the purpose, the invention provides the following technical scheme:
a rapid ceramic sintering device comprises a furnace body, an observation window arranged on one side of the furnace body, a pressurizing assembly and a temperature measuring assembly which are arranged in the furnace body, an electrifying assembly and an insulating assembly, wherein a graphite mold is arranged at the center of an inner cavity of the furnace body, and a graphite soft felt which is arranged in an S shape and is provided with a sample is arranged in the graphite mold;
the electrifying assembly is arranged above and below the graphite soft felt and matched with the BN side plate and is used for electrifying and heating a sample placed in the graphite soft felt;
the pressurizing assembly is arranged at the upper end and the lower end of the furnace body and is used for pressing and forming a sample;
the insulating assembly is respectively arranged on the graphite soft felt and the graphite die, the pressure head on the stainless steel pressure head of the pressurizing assembly and the pressure head on the graphite, the pressure head under the stainless steel pressure head of the pressurizing assembly and the pressure head under the graphite, the graphite pressure head and the graphite die, and the graphite pressure head and the graphite die are arranged between the pressure head and the graphite die and used for electrical insulation, so that the current is ensured to only flow through the graphite soft felt and not flow through the graphite die, the stainless steel pressure head and the stainless steel pressure head, the current short circuit in the furnace body can not be caused, and the graphite soft felt is ensured to be only subjected to power-on heating.
As a further scheme of the invention, the electrifying assembly comprises an upper graphite pressure head, copper electrodes, a power supply and a lower graphite pressure head, wherein the upper graphite pressure head and the lower graphite pressure head are respectively arranged above and below the soft graphite felt and are in contact with the soft graphite felt, the power supply is arranged outside the furnace body, two ends of the power supply are respectively connected with the copper electrodes, the other ends of the two copper electrodes respectively penetrate through the furnace body to be electrically connected with the upper graphite pressure head and the lower graphite pressure head, and the copper electrodes and the furnace body are insulated and sealed by polytetrafluoroethylene.
As a further scheme of the invention, the pressurizing assembly comprises a hydraulic control element, a pressure sensor, a stainless steel upper pressure head and a stainless steel lower pressure head, wherein the stainless steel upper pressure head is arranged at the upper end part of the furnace body, the bottom end of the stainless steel upper pressure head is connected with the upper end surface of the graphite upper pressure head, the stainless steel lower pressure head is arranged at the lower end part of the furnace body, the top end of the stainless steel lower pressure head is fixedly connected with the graphite lower pressure head, the bottom end of the stainless steel lower pressure head is fixedly connected with the output end of the hydraulic control element arranged outside the furnace body, and the pressure sensor is arranged at the connection part of the hydraulic control element and the stainless steel lower pressure head and is used for detecting the pressure applied by the hydraulic control element.
As a further scheme, the insulation assembly comprises a BN side plate, a BN upper plate, a BN lower plate, and a BN upper insulation sleeve and a BN lower insulation sleeve which are arranged on a graphite upper pressure head and a graphite lower pressure head, wherein the BN side plate is arranged at the joint of the inner wall of a graphite die and a graphite soft felt, the BN upper plate and the BN lower plate are respectively laid on the upper end surface and the lower end surface of the graphite die, and central holes matched with the graphite upper pressure head and the graphite lower pressure head are formed in the BN upper plate and the BN lower plate.
As a further scheme of the invention, the ends of the BN upper insulating sleeve and the BN lower insulating sleeve are respectively provided with a thread groove matched with the stainless steel upper pressure head and the stainless steel lower pressure head.
As a further scheme of the invention, the temperature measuring component comprises an infrared thermometer and a thermocouple arranged on the inner wall of the BN side plate, a through hole is arranged at the equal height position of the BN side plate and the graphite mold, the through hole corresponds to the sensing end of the infrared thermometer arranged outside the observation window, and the other end of the infrared thermometer is electrically connected with a computer for obtaining the temperature and time curve of the graphite soft felt in real time.
As a further scheme of the invention, the BN side plate is formed by splicing four petals and encloses a square hole groove for placing the graphite soft felt and the sample.
As a still further aspect of the invention, the sample is made of ceramic powder, and the ceramic powder is one or more of oxide or carbide, nitride, boride and ceramic-metal composite material.
A sintering method of a rapid sintering ceramic device comprises the following steps:
1) pressing ceramic powder into a sample green body with a certain shape under the pressure of 200-500 MPa, then placing the sample green body on a graphite soft felt, wrapping the sample by the graphite soft felt to form an S shape, and placing the sample in a graphite mold;
2) respectively contacting the graphite upper pressure head and the graphite lower pressure head with the graphite soft felt, and connecting the graphite upper pressure head and the graphite lower pressure head with a power supply through copper electrodes;
3) vacuumizing the furnace to below 10Pa, turning on a power switch to electrify the graphite soft felt, and adjusting the current to ensure that the temperature of the graphite soft felt quickly reaches a preset value, wherein the power voltage range is 10-30V, and the current range is 20-50A;
4) after the temperature is constant, keeping electrifying for 5-30 s;
5) in the heat preservation process, 0-50 MPa of pressure is applied, then a power supply is disconnected, and the temperature is reduced at a certain rate.
As a further scheme of the invention, a sample is wrapped between S-shaped stacked graphite soft felts, when the sample to be sintered is conductive or can react with graphite at high temperature, and the sintering temperature is less than or equal to 1200 ℃, 0.5mm of alumina fiber paper is adopted between the sample and the graphite soft felts for insulation, and the sample, the fiber paper and the graphite soft felts are stacked into an S shape and placed in a graphite mold; when the sample to be sintered is conductive or can react with graphite at high temperature, the sintering temperature is higher than 1200 ℃, and BN powder is sprayed on the surface of the sample to insulate the sample from the graphite soft felt.
Compared with the prior art, the invention has the beneficial effects that:
1. compared with the traditional sintering method, the method does not need to heat the furnace body, has high heating speed, high sintering temperature and short period, greatly improves the production efficiency and reduces the energy consumption;
2. compared with SPS technology, the present invention needs no expensive DC pulse power source, and has applied current of several ten amperes far less than that of hundreds to thousands of great current. Meanwhile, the method does not need to heat the die, heat is directly applied to the samples through heat conduction, the heating speed is high, the energy utilization rate is high, a plurality of samples can be sintered simultaneously, high-throughput preparation is realized, the energy consumption is low, and the device is simple.
3. Compared with the flash firing technology, the method has no special selectivity requirement on materials, the sample does not need to be preheated to a certain temperature by a furnace, the sintering period is short, and the simultaneous preparation of multiple samples can be realized.
In a word, the method is simple to operate, efficient, easy to implement and strong in universality, ceramic sintering technologies are enriched, and the obtained ceramic is high in densification degree.
Drawings
FIG. 1 is a schematic diagram of a rapid sintering apparatus for use in the present invention.
FIG. 2 is a graph illustrating temperature versus time in the present invention.
FIG. 3 shows Al obtained in example 1 of the present invention2O3And (4) microstructure topography.
FIG. 4 shows La obtained in example 4 of the present invention2Zr2O7And (4) microstructure topography.
FIG. 5 shows the high-entropy oxide ceramic (La) obtained in example 5 of the present invention0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7And (4) microstructure topography.
FIG. 6 is a TiC microstructure topography obtained in example 6 of the present invention.
In the figure, 1, a stainless steel upper pressure head; 2. BN is provided with an insulating sleeve; 3. pressing a graphite upper pressing head; 4. a copper electrode; 5. BN upper plate; 6. a power source; 7. a graphite mold; 8. BN side plate; 9. a BN lower plate; 10. a graphite lower pressure head; 11. a hydraulic control element; 12. a pressure sensor; 13. a stainless steel lower pressure head; 14. BN lower insulating sleeve; 15. a sample; 16. a thermocouple; 17. an observation window; 18. graphite soft felt; 19. a furnace body; 20. an infrared thermometer.
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 figure 1, the invention provides a rapid ceramic sintering device, which comprises a furnace body 19, an observation window 17 arranged on one side of the furnace body 19, a pressurizing assembly and a temperature measuring assembly arranged in the furnace body 19, an electrifying assembly and an insulating assembly, wherein a graphite mold 7 is arranged at the center of an inner cavity of the furnace body 19, and a graphite soft felt 18 which is arranged in an S shape and is provided with a sample 15 is arranged in the graphite mold 7;
the electrifying assembly is arranged above and below the graphite soft felt 18 and matched with the BN side plate 8 and is used for electrifying and heating the sample 15 placed in the graphite soft felt 18;
the pressurizing assembly is arranged at the upper end and the lower end of the furnace body 19 and is used for pressing and forming the sample 15;
the insulating components are respectively arranged between the graphite soft felt 18 and the graphite die 7, between the stainless steel upper pressure head 1 and the graphite upper pressure head 3 of the pressurizing components, between the stainless steel lower pressure head 13 and the graphite lower pressure head 10 of the pressurizing components, between the graphite upper pressure head 3 and the graphite die 7, and between the graphite lower pressure head 10 and the graphite die 7, and are used for electrical insulation, so that the current is ensured to only flow through the graphite soft felt 18, but not flow through the graphite die 7, the stainless steel upper pressure head 1 and the stainless steel lower pressure head 13, and the current short circuit in the furnace body is not caused, and the graphite soft felt 18 is ensured to be only electrified and heated;
the electrifying component comprises a graphite upper pressure head 3, a copper electrode 4, a power supply 6 and a graphite lower pressure head 10, wherein the graphite upper pressure head 3 and the graphite lower pressure head 10 are respectively arranged above and below a graphite soft felt 18 and are in contact with the graphite soft felt 18, the power supply 6 is arranged outside a furnace body 19, two ends of the power supply are respectively connected with the copper electrode 4, the other ends of the two copper electrodes 4 respectively penetrate through the furnace body 19 and the graphite upper pressure head 3 and the graphite lower pressure head 10 to be electrically connected, and the copper electrode and the furnace body are insulated and sealed by polytetrafluoroethylene.
The pressurizing assembly comprises a hydraulic control element 11, a pressure sensor 12, a stainless steel upper pressure head 1 and a stainless steel lower pressure head 13, the stainless steel upper pressure head 1 is arranged at the upper end part of the furnace body 19, the bottom end of the stainless steel upper pressure head is connected with the upper end surface of the graphite upper pressure head 3, the stainless steel lower pressure head 13 is arranged at the lower end part of the furnace body 19, the top end of the stainless steel lower pressure head is fixedly connected with the graphite lower pressure head 10, the bottom end of the stainless steel lower pressure head 13 is fixedly connected with the output end of the hydraulic control element 11 arranged outside the furnace body 19, and the pressure sensor 12 is arranged at the joint of the hydraulic control element 11 and the stainless steel lower pressure head 13 and is used for detecting the pressure applied by the hydraulic control element 11;
the insulation assembly comprises a BN side plate 8, a BN upper plate 5, a BN lower plate 9, and a BN upper insulation sleeve 2 and a BN lower insulation sleeve 14 which are arranged on the graphite upper pressure head 3 and the graphite lower pressure head 10, wherein the BN side plate 8 is arranged at the joint of the inner wall of the graphite mold 7 and the graphite soft felt 18, the BN upper plate 5 and the BN lower plate 9 are respectively laid on the upper end surface and the lower end surface of the graphite mold 7, and the BN upper plate 5 and the BN lower plate 9 are provided with central holes matched with the graphite upper pressure head 3 and the graphite lower pressure head 10; when the device works, the insulating assembly is used for ensuring that current only flows through the graphite soft felt 18, but not flows through the graphite die 7, the stainless steel upper pressure head 1 and the stainless steel lower pressure head 13, and the current short circuit in the furnace body 19 can not be caused, so that the electrifying assembly is ensured to only electrify and heat the graphite soft felt 18;
the end parts of the BN upper insulating sleeve 2 and the BN lower insulating sleeve 14 are respectively provided with a thread groove matched with the stainless steel upper pressure head 1 and the stainless steel lower pressure head 13;
the temperature measuring component comprises an infrared thermometer 20 and a thermocouple 16 arranged on the inner wall of the BN side plate 8, a through hole is formed at the equal height position of the BN side plate 8 and the graphite mold 7, the through hole corresponds to the sensing end of the infrared thermometer 20 arranged outside the observation window 17, and the other end of the infrared thermometer 20 is electrically connected with a computer for obtaining the temperature and time curve of the graphite soft felt 18 in real time; the temperature in the furnace body 19 is measured by an infrared thermometer 20 and a thermocouple 16 simultaneously, or can be used independently, the temperature range of the infrared thermometer 20 used in the experiment is 1000-3200 ℃, the temperature of the sample 15 is recorded by the thermocouple 16, and the thermocouple 16 is connected with a temperature control meter and transmits data to a computer;
the BN side plate 8 is formed by splicing four petals and encloses a square hole groove for placing the graphite soft felt 18 and the sample 15;
sample 15 was made from ceramic powder; the ceramic powder is one or more of oxide or carbide, nitride, boride and ceramic-metal composite material.
Example 1:
in this embodiment, a rapid high temperature sintering Al2O3The new method is carried out according to the following steps:
a. firstly 30nm of Al2O3The powder was mixed with 3 wt.% aqueous PVA solution and ground to homogeneity and then pressed under a pressure of 400MPa to a size of 20X 4mm3Al of (2)2O3Green compact, initial density of 50%;
b. pre-burning the green body prepared in the step a in the air at 600 ℃ for 1h to remove organic PVA;
c. placing the 5 blanks obtained in the step b between S-shaped stacked graphite soft felts 18 with the length of 150mm, the width of 20mm and the thickness of 3mm, enclosing to form an S shape, and placing the S shape into a square hole groove of a BN side plate 8 in a graphite mold 7; then the furnace is vacuumized to below 10 Pa;
d. electrifying to make current quickly reach 35A, heating the sample to 1800 deg.C at 1000 deg.C/min, keeping the temperature for 20s, and cooling to room temperature at the rate to obtain Al2O3And (5) fast high-temperature sintering.
e. The density of the obtained blank is measured by adopting an Archimedes method, and the density of the blank is calculated to obtain 92%.
The change curve of the temperature with time recorded in example 1 of the present invention is shown in fig. 2; the microstructure is shown in fig. 3.
Example 2:
this example differs from example 1 in that: the initial alumina particles have a size of 500nm, a current of 40A, a sintering temperature of 2000 ℃ and other parameters and steps similar to those of example 1, and the measured density is as high as 95%.
Example 3:
this example differs from example 1 in that: sample 15 dimensions phi 12X 4mm2The graphite soft felt 18 has the size of 150mm multiplied by 20mm multiplied by 5mm, the current is 35A, the sintering temperature is 1800 ℃, and other parameters, steps and implementation are carried outThe same as in example 1, the density was measured up to 95%.
Example 4:
the composite oxide ceramic La with the ceramic powder of 30nm selected in the example2Zr2O7Sample size of phi 6X 4mm2The number of the samples is 10, and the size of the graphite soft felt is 100 multiplied by 15 multiplied by 4mm3The applied current is 40A, the temperature is 1900 ℃, the heat preservation time is 22s, and the heating and cooling rate is 750 ℃/min. Other parameters and procedures were the same as in example 1, with a ceramic densification of up to 97%, the microstructure of which is shown in FIG. 4.
Example 5:
the ceramic powder selected in the example is a high-entropy oxide ceramic (La) with the grain size of 30nm0.2Nd0.2Sm0.2Eu0.2Gd0.2)2Zr2O7Sample size of phi 6X 4mm2The graphite soft felt has the size of 120 multiplied by 15 multiplied by 4mm3The number of samples was 6, the applied current was 35A, the temperature was 1800 ℃ and the heating and cooling rates were 400 ℃/min. Other parameters and procedures were the same as in example 1, with a ceramic densification of up to 98%, the microstructure being shown in FIG. 5.
Example 6:
the ceramic powder selected in this example was 1 μm TiC, which is different from example 1 in that the ceramic powder was not mixed with PVA aqueous solution and it was not calcined at 600 ℃ to remove organic matter. And (3) spraying BN insulation on the surface of the TiC blank to ensure that the graphite soft felt generates enough joule heat. The sample size is phi 12 multiplied by 4mm2The graphite soft felt has the size of 150 multiplied by 20 multiplied by 3mm3The number of the heating elements is 5, the magnitude of applied current is 48A, the temperature is 2300 ℃, the heating and cooling rate is 1500 ℃/min, and the magnitude of applied pressure is 27 MPa. The ceramic density was as high as 94% and the microstructure is shown in figure 6.
Example 7:
the ceramic powder selected in this example was 1 μm Si3N4Except that the ceramic powder is not required to be mixed with the PVA water solution and is not required to be pre-sintered at 600 ℃ to remove organic matters. The sample size is 20mm multiplied by 3mm, the number is 4, the graphite soft felt size is 150mm multiplied by 20mm multiplied by 3mm3The applied current is 35A, the temperature is 1800 ℃, the heating and cooling rate is 1000 ℃/min, the applied pressure is 30MPa, and the ceramic density is up to 95%.
Example 8:
the ceramic powder selected in this example was 1 μm TiB2Unlike example 1, the ceramic powder was not mixed with the aqueous PVA solution nor calcined at 600 ℃ to remove the organic matter. TiB2The surface of the blank is sprayed with BN insulation to ensure that the graphite soft felt generates enough joule heat. The graphite soft felt has the size of 160 multiplied by 20 multiplied by 3mm3The size of the sample is 10mm multiplied by 3mm, the number of the samples is 5, the magnitude of the applied current is 45A, the temperature is 2200 ℃, the heating and cooling rate is 1500 ℃/min, the magnitude of the applied pressure is 28MPa, and the density of the ceramic is as high as 94%.
Example 9:
the ceramic powder selected in this example was 1 μm Li1.5Al0.5Ge1.5(PO4)3(LAGP), unlike example 1, the LAGP blank was isolated from the graphite felt by alumina fiber paper. The fiber paper and the graphite soft felt are closely contacted and arranged in an S-shaped lamination. The graphite soft felt has the size of 150 multiplied by 20 multiplied by 2mm3The applied current is 20A, the temperature is 1000 ℃, the heating and cooling rate is 2000 ℃/min, no pressure is required to be applied, and the ceramic density is as high as 94%.
The working principle of the invention is as follows: when the device works, ceramic powder is pressed into a sample 15 green body with a certain size under a certain pressure, the sample 15 is placed between the graphite soft felts 18 which are stacked in an S shape in a furnace body 19, a power supply 6 is started, direct current is applied to the graphite soft felts 18 through a copper electrode 4, after the temperature is stable, a pressurizing assembly applies pressure, the sample 15 is rapidly sintered within a plurality of seconds under the action of Joule heat conduction and pressure, and the sample 15 is rapidly cooled to room temperature after power failure; the ceramic adopts current thermal effect and heat conduction to realize faster heating rate and simultaneously avoid large heat loss; sample 15 bypasses the low temperature slow heating stage at an ultra-fast heating rate, thereby reducing particle growth, maintaining a higher sintering driving force, and increasing densification rate; the method has the advantages of simple operation, high efficiency, easy implementation, strong universality, enrichment of ceramic sintering technology, higher densification degree of the obtained ceramic and wider applicability. It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (10)

1.一种快速烧结陶瓷装置，包括炉体(19)、开设在炉体(19)一侧的观察窗(17)以及设置在炉体(19)内的加压组件和测温组件，其特征在于：还包括通电组件与绝缘组件，所述炉体(19)内腔中心处设有石墨模具(7)，所述石墨模具(7)内设有呈S形设置并放置有样品(15)的石墨软毡(18)；1. A rapid sintering ceramic device, comprising a furnace body (19), an observation window (17) provided on one side of the furnace body (19), and a pressurizing component and a temperature measuring component arranged in the furnace body (19), which It is characterized in that: it also includes an energizing component and an insulating component, a graphite mold (7) is arranged at the center of the inner cavity of the furnace body (19), and a sample (15) is arranged in the graphite mold (7) in an S-shape. ) of graphite soft felt (18); 所述通电组件设置在石墨软毡(18)上下方并与BN侧板(8)相配合，用于对所述石墨软毡(18)内放置的所述样品(15)通电加热；The electrification components are arranged above and below the soft graphite felt (18) and cooperate with the BN side plate (8), and are used for electrifying and heating the sample (15) placed in the soft graphite felt (18); 所述加压组件，设置在所述炉体(19)的上下端，用于对所述样品(15)压制成型；The pressing components are arranged at the upper and lower ends of the furnace body (19), and are used for pressing and forming the sample (15); 所述绝缘组件，分别设置在石墨软毡(18)与石墨模具(7)，加压组件不锈钢上压头(1)和石墨上压头(3)，加压组件不锈钢下压头(13)和石墨下压头(10)，石墨上压头(3)与石墨模具(7)，石墨下压头(10)和石墨模具(7)之间，用于电绝缘，以确保电流只流经石墨软毡(18)，而不流经石墨模具(7)和不锈钢上压头(1)以及不锈钢下压头(13)，也不会引起炉体内电流短路，从而保证只对石墨软毡(18)通电加热。The insulating components are respectively arranged on the graphite soft felt (18) and the graphite mold (7), the stainless steel upper indenter (1) and the graphite upper indenter (3) of the pressing component, and the stainless steel lower indenter (13) of the pressing component and graphite lower indenter (10), graphite upper indenter (3) and graphite mold (7), graphite lower indenter (10) and graphite mold (7) for electrical insulation to ensure that current only flows through The graphite soft felt (18) does not flow through the graphite mold (7) and the stainless steel upper indenter (1) and the stainless steel lower indenter (13), and will not cause a short circuit in the furnace body, thus ensuring that only the graphite soft felt ( 18) Electric heating. 2.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述通电组件包括石墨上压头(3)、铜电极(4)、电源(6)和石墨下压头(10)，所述石墨上压头(3)和石墨下压头(10)分别设置在石墨软毡(18)上下方并与石墨软毡(18)相接触，所述电源(6)设置在炉体(19)外，其两端分别连接有铜电极(4)，两个所述铜电极(4)另一端分别穿过炉体(19)与石墨上压头(3)和石墨下压头(10)电性连接，所述铜电极(4)与炉体(19)之间用聚四氟乙烯绝缘并密封。2. A rapid sintering ceramic device according to claim 1, characterized in that: the energization component comprises a graphite upper indenter (3), a copper electrode (4), a power source (6) and a graphite lower indenter (10). ), the graphite upper indenter (3) and the graphite lower indenter (10) are respectively arranged above and below the graphite soft felt (18) and are in contact with the graphite soft felt (18), and the power supply (6) is arranged in the furnace Outside the body (19), copper electrodes (4) are connected at both ends, and the other ends of the two copper electrodes (4) pass through the furnace body (19) and the graphite upper indenter (3) and the graphite lower indenter respectively. (10) Electrical connection, the copper electrode (4) and the furnace body (19) are insulated and sealed with polytetrafluoroethylene. 3.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述加压组件包括液压控制元件(11)、压力传感器(12)、不锈钢上压头(1)和不锈钢下压头(13)，所述不锈钢上压头(1)设置在炉体(19)上端部，其底端与石墨上压头(3)上端面相连接，所述不锈钢下压头(13)设置在炉体(19)下端部，其顶端与石墨下压头(10)固定连接，所述不锈钢下压头(13)底端与设置在炉体(19)外的液压控制元件(11)输出端固定连接，所述压力传感器(12)设置在液压控制元件(11)与不锈钢下压头(13)的连接处，用于对液压控制元件(11)施加的压力进行检测。3. A rapid sintering ceramic device according to claim 1, characterized in that: the pressurizing component comprises a hydraulic control element (11), a pressure sensor (12), a stainless steel upper pressure head (1) and a stainless steel downward pressure Head (13), the stainless steel upper indenter (1) is arranged on the upper end of the furnace body (19), and its bottom end is connected with the upper end face of the graphite upper indenter (3), and the stainless steel lower indenter (13) is arranged on the upper end of the upper indenter (3). The lower end of the furnace body (19), the top of which is fixedly connected with the graphite lower pressure head (10), the bottom end of the stainless steel lower pressure head (13) and the output end of the hydraulic control element (11) arranged outside the furnace body (19) Fixed connection, the pressure sensor (12) is arranged at the connection between the hydraulic control element (11) and the stainless steel lower pressure head (13), and is used for detecting the pressure exerted by the hydraulic control element (11). 4.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述绝缘组件包括BN侧板(8)、BN上板(5)、BN下板(9)和设置在石墨上压头(3)与石墨下压头(10)上的BN上绝缘套(2)和BN下绝缘套(14)，所述BN侧板(8)设置在石墨模具(7)内壁与石墨软毡(18)的连接处，所述BN上板(5)和BN下板(9)分别铺设在石墨模具(7)上下端面，所述BN上板(5)和BN下板(9)上开设有与石墨上压头(3)和石墨下压头(10)相配合的中心孔。4. A rapid sintering ceramic device according to claim 1, characterized in that: the insulating component comprises a BN side plate (8), a BN upper plate (5), a BN lower plate (9), and a BN side plate (8), a The BN upper insulating sleeve (2) and the BN lower insulating sleeve (14) on the indenter (3) and the graphite lower indenter (10), the BN side plate (8) is arranged on the inner wall of the graphite mold (7) and the graphite soft The junction of the felt (18), the BN upper plate (5) and the BN lower plate (9) are respectively laid on the upper and lower end faces of the graphite mold (7), the BN upper plate (5) and the BN lower plate (9) A central hole matched with the graphite upper indenter (3) and the graphite lower indenter (10) is opened. 5.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述BN上绝缘套(2)和BN下绝缘套(14)端部分别开设有与不锈钢上压头(1)、不锈钢下压头(13)相配合的螺纹槽。5. A rapid sintering ceramic device according to claim 1, characterized in that: the ends of the BN upper insulating sleeve (2) and the BN lower insulating sleeve (14) are respectively provided with a stainless steel upper indenter (1) , The stainless steel lower pressure head (13) is matched with the thread groove. 6.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述测温组件包括红外测温仪(20)和设置在BN侧板(8)内壁上的热电偶(16)，所述BN侧板(8)和石墨模具(7)等高位置处开设有一个通孔，所述通孔与设置在观察窗(17)外的红外测温仪(20)感应端相对应，所述红外测温仪(20)另一端与计算机电性连接，用以实时获得石墨软毡(18)的温度与时间曲线。6 . The rapid sintering ceramic device according to claim 1 , wherein the temperature measuring component comprises an infrared thermometer ( 20 ) and a thermocouple ( 16 ) arranged on the inner wall of the BN side plate ( 8 ). 7 . , a through hole is opened at the height position of the BN side plate (8) and the graphite mold (7), and the through hole corresponds to the induction end of the infrared thermometer (20) arranged outside the observation window (17). , the other end of the infrared thermometer (20) is electrically connected with the computer, so as to obtain the temperature and time curve of the graphite soft felt (18) in real time. 7.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述BN侧板(8)由四瓣拼接而成，围成一个方形孔槽，用于对所述石墨软毡(18)和样品(15)进行放置。7 . The rapid sintering ceramic device according to claim 1 , wherein the BN side plate ( 8 ) is formed by splicing four petals and encloses a square hole groove, which is used for the graphite soft felt. 8 . (18) and the sample (15) are placed. 8.根据权利要求1所述的一种快速烧结陶瓷装置，其特征在于：所述样品(15)由陶瓷粉末制成,所述陶瓷粉末为氧化物、碳化物、氮化物、硼化物以及陶瓷金属复合材料中的一种或多种复合。8. A rapid sintering ceramic device according to claim 1, characterized in that: the sample (15) is made of ceramic powder, and the ceramic powder is oxide, carbide, nitride, boride and ceramic One or more composites of metal composites. 9.根据权利要求1-8任一所述的一种快速烧结陶瓷装置的烧结方法，其特征在于，包括以下几个步骤；9. The sintering method for a rapid sintering ceramic device according to any one of claims 1-8, characterized in that it comprises the following steps; 1)陶瓷粉末在200～500MPa的压力下压制成具有一定形状的样品(15)生坯，然后将样品(15)生坯放置于石墨软毡(18)上，石墨软毡(18)包裹着样品(15)围成S形放置在石墨模具(7)内；1) The ceramic powder is pressed under a pressure of 200 to 500 MPa to form a green body of a sample (15) having a certain shape, and then the green body of the sample (15) is placed on a soft graphite felt (18), and the soft graphite felt (18) is wrapped The sample (15) is placed in the graphite mold (7) in an S shape; 2)将石墨上压头(3)和石墨下压头(10)分别与石墨软毡(18)接触，并通过铜电极(4)与电源(6)相连；2) the graphite upper indenter (3) and the graphite lower indenter (10) are respectively contacted with the graphite soft felt (18), and are connected with the power supply (6) through the copper electrode (4); 3)炉子抽真空至10Pa以下，然后打开电源(6)开关给石墨软毡(18)通电，调节电流使石墨软毡(18)温度迅速达到预定值，所述电源(6)电压范围为10-30V，电流范围为20-50A；3) The furnace is evacuated to below 10Pa, and then the power supply (6) switch is turned on to energize the graphite soft felt (18), and the current is adjusted so that the temperature of the graphite soft felt (18) quickly reaches a predetermined value, and the voltage range of the power supply (6) is 10 -30V, the current range is 20-50A; 4)温度恒定后，保持通电5～30s；4) After the temperature is constant, keep the power on for 5-30s; 5)在保温过程中，施加0～50MPa压力，随后断开电源(6)，按一定速率进行降温。5) During the heat preservation process, a pressure of 0 to 50 MPa is applied, then the power supply (6) is disconnected, and the temperature is lowered at a certain rate. 10.根据权利要求9所述的一种快速烧结陶瓷装置的烧结方法，其特征在于：在步骤1)中，样品(15)被包裹在S形叠放的石墨软毡(18)之间，当待烧结样品(15)导电或者高温下会与石墨反应，且烧结温度≤1200℃时，样品(15)与石墨软毡(18)之间采用0.5mm氧化铝纤维纸使其绝缘，样品(15)、纤维纸与石墨软毡(18)叠成S形放置到石墨模具(7)；当待烧结样品(15)导电或者高温下会与石墨反应，且烧结温度＞1200℃时，样品(15)表面喷涂BN粉体，使其与石墨软毡(18)绝缘。10. The sintering method for a rapid sintering ceramic device according to claim 9, characterized in that: in step 1), the sample (15) is wrapped between the S-shaped stacked graphite soft felts (18), When the sample (15) to be sintered conducts electricity or reacts with graphite at high temperature, and the sintering temperature is less than or equal to 1200°C, 0.5mm alumina fiber paper is used between the sample (15) and the graphite soft felt (18) to insulate the sample (15). 15), the fiber paper and the graphite soft felt (18) are stacked in an S shape and placed on the graphite mold (7); when the sample (15) to be sintered is conductive or will react with graphite at high temperature, and the sintering temperature is > 1200 ° C, the sample ( 15) Spray BN powder on the surface to insulate it from the graphite soft felt (18).
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