CN111981847A - Pressure-assisted induction heating vacuum atmosphere flash sintering device - Google Patents

Pressure-assisted induction heating vacuum atmosphere flash sintering device Download PDF

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Publication number
CN111981847A
CN111981847A CN202010723873.0A CN202010723873A CN111981847A CN 111981847 A CN111981847 A CN 111981847A CN 202010723873 A CN202010723873 A CN 202010723873A CN 111981847 A CN111981847 A CN 111981847A
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flash
pressure
induction heating
furnace body
burning
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张新房
梁艺涵
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University of Science and Technology Beijing USTB
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University of Science and Technology Beijing USTB
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00—Furnaces of a kind not covered by any preceding group
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D11/00—Arrangement of elements for electric heating in or on furnaces
    • F27D11/06—Induction heating, i.e. in which the material being heated, or its container or elements embodied therein, form the secondary of a transformer
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00—Cooling of furnaces or of charges therein
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00—Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/06—Forming or maintaining special atmospheres or vacuum within heating chambers
    • F27D2007/066—Vacuum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00—Cooling of furnaces or of charges therein
    • F27D2009/0002—Cooling of furnaces
    • F27D2009/001—Cooling of furnaces the cooling medium being a fluid other than a gas
    • F27D2009/0013—Cooling of furnaces the cooling medium being a fluid other than a gas the fluid being water
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27—FURNACES; KILNS; OVENS; RETORTS
    • F27M—INDEXING SCHEME RELATING TO ASPECTS OF THE CHARGES OR FURNACES, KILNS, OVENS OR RETORTS
    • F27M2003/00—Type of treatment of the charge
    • F27M2003/04—Sintering

Abstract

The invention relates to the field of new material preparation, and provides a pressure-assisted induction heating vacuum atmosphere flash sintering device which comprises a furnace body, a pressure system, a flash combustion system, an induction heating system, a cooling system and a vacuum system; the pressure system comprises an upper pressure head and a movable lower pressure head, and an upper electrode and a lower electrode are respectively arranged at the end parts of the upper pressure head and the lower pressure head and provide pressure for flash burning samples; the flash burning system provides a flash burning loop; the induction heating system provides heating and heat preservation; the cooling system cools the furnace body; the vacuum system vacuumizes the furnace body. The invention overcomes the inherent defects in the traditional flash sintering technology, can flexibly select a flash power supply according to the electrical properties of the flash sintered material to trigger thermal runaway, thereby realizing the maximum densification level and the fine regulation and control of the microstructure of a sample, and having universality on metal and ceramic materials; the invention can easily realize the pressure assistance in the flash combustion process and provide a new preparation means for the research field.

Description

Pressure-assisted induction heating vacuum atmosphere flash sintering device
Technical Field
The invention relates to the technical field of new material preparation, in particular to a pressure-assisted induction heating vacuum atmosphere flash sintering device.
Background
Since 2010 flash sintering (or flash sintering or flash firing) was proposed, it has been appliedFor a variety of materials, including ionic conductors such as Yttria Stabilized Zirconia (YSZ) and Gadolinium Doped Ceria (GDC); semiconductors such as zinc oxide (ZnO) and silicon carbide (SiC); and certain types of electronic conductors and insulators, e.g. Co2MnO4Strontium titanate (SrTiO)3) And alumina (Al)2O3). The most obvious advantage of flash sintering over conventional sintering processes is that it greatly reduces the time, temperature and energy required for ceramic densification, meaning that it has significant implications and application prospects in terms of industrial and environmental benefits.
In recent years, the realization of flash sintering using novel experimental equipment has attracted attention from the international scientific and technical communities, such as flash discharge plasma sintering (FSPS), flash sintering forging, and non-contact flash sintering. The FSPS realizes flash sintering of high-melting-point carbide, nitride and boride which are extremely difficult to sinter by reforming commercial discharge plasma equipment and applying extremely high pulse direct current; the non-contact flash sintering adopts plasma as an electrode, so that the physical contact between the electrode and a sample is avoided, and the problems that a platinum electrode is expensive, current flows unevenly to generate hot spots and the like in the conventional flash sintering method are solved. These emerging technologies offer the possibility of flash sintering to be extended to industrial applications.
Nevertheless, both in conventional flash sintering and with these new techniques, the green body must be subjected to a series of pre-treatments to ensure it has sufficient mechanical strength for flash sintering experiments. These pretreatments typically include mixing the powder with a binder or sintering aid, burning off the binder in a conventional furnace, or presintering by SPS in the case of FSPS. These additional pre-treatment processes deprive flash sintering of its inherent advantages of energy saving and rapid processing, which runs counter to its original purpose of development.
Based on the application prospect of flash sintering technology in the field of new material preparation, related scientific and technical papers and patents are also successively published and applied.
Patents (US9334194B2, US8940220B2) describe in detail the connotation, method of operation and basic research equipment for flash sintering of ceramic materials; the patent (EP2691551B1) reports a method for manufacturing complex-shaped parts based on flash sintering technology; patent (JP5562857B2) reports a method for preparing dense iodoapatite based on flash sintering technique; patent (US9212424B1) reports a method of flash sintering by flame heating; the patent (US20150329430a1) reports a process for the preparation of multilayer ceramics based on flash sintering technology; patent (CN108558398A) reports a method for pulse discharge room temperature flash sintering of nano ceramic material; patent (CN106630974A) reports a flash sintering method for rapidly sintering ceramics at low temperature in a tube furnace environment and the ceramics and the device; patents (CN108645204A, CN208419576U) report a sintering furnace coupling hot-pressing sintering and flash-firing technologies; patent (CN210070583U) reports a sintering furnace coupling microwave heating technology and flash firing technology. The patent (CN110577399A) reports a multi-field coupling flash sintering system based on induction heating, which describes the characteristics of each module and the interaction relationship between the modules macroscopically, but does not mention specific equipment structure, and can only apply the pressure of 20-50 MPa, and does not meet the conditions that some higher pressure needs to be applied. Patent (CN210070584U) reports a sintering furnace induction auxiliary heating device for flash firing of ceramic crystals, which also uses induction heating as a rapid preheating means for flash firing samples while applying an axial pressure, but the patent does not describe the flash firing samples and the mold further. However, the key to flash firing technology is forcing current to flow directly through the sintered body, inducing thermal runaway, thereby increasing the diffusion rate of the species and achieving rapid densification. The relative spatial positions of the sample, the die and the ram (which may also serve as electrodes) are therefore of particular importance, and flash firing techniques cannot be effectively employed unless they are specifically defined.
Disclosure of Invention
The technical problems solved by the invention are as follows:
in the flash sintering process, the preheating of the sample does not require the use of the more complex equipment mentioned in the above-mentioned patent and consumes a lot of energy, and since the problem of non-uniformity of the current cannot be solved effectively in academic or technical circles for a while, the flash sintered sample is usually very small, and for cylindrical samples, both the diameter and the height are around 10mm, so that only effective local heating of the sample is required. The present invention provides a new system and method for performing pressure assisted flash sintering without any pretreatment. For a ceramic sample (the resistance temperature coefficient is negative), energy can be concentrated in an electrode-sample-electrode area or a die-sample area by medium-frequency or high-frequency induction heating, so that ultra-fast and energy-saving local heating is realized, and the ceramic can reach the flash firing temperature quickly; for metal or metal-like materials with good room-temperature conductivity, resistance heating is directly realized at room temperature by utilizing a special die and an electrode structure, and thermal runaway is initiated to realize flash firing. Therefore, the loose powder can be subjected to flash firing in situ in a specially-structured die with the assistance of pressure, no additional pretreatment is required to be carried out on the ceramic green body, the pressure can reach 2GPa at most, and the flash firing time is less than 30 s. The invention can be used for the research and production of various advanced materials of ceramic matrix and metal matrix. However, the invention is particularly suitable for the flash sintering preparation of various types of nuclear fuel pellets based on the limitations of the conventional fuel pellet sintering process in the nuclear fuel industry.
Aiming at the defects of the prior art, the invention adopts the following technical scheme:
a pressure-assisted induction heating vacuum atmosphere flash sintering device is mainly used for flash sintering preparation of various nuclear fuel pellets, materials of the various nuclear fuel pellets comprise uranium dioxide, uranium carbide, uranium nitride, uranium silicide and composite materials taking the uranium dioxide, the uranium carbide, the uranium nitride and the uranium silicide as matrixes, and the pressure-assisted induction heating vacuum atmosphere flash sintering device is a brand-new nuclear fuel pellet sintering method. The device comprises a furnace body, a pressure system, a flash burning system, an induction heating system, a cooling system and a vacuum system;
the pressure system comprises an upper pressure head and a movable lower pressure head, wherein the upper pressure head is fixedly arranged relative to the top of the furnace body; the end part of the upper pressure head is provided with an upper electrode, and the end part of the lower pressure head is provided with a lower electrode; when the upper pressing head and the lower pressing head move relatively, the upper electrode and the lower electrode are driven to provide pressure for flash burning samples;
the flash burning system comprises a flash burning power supply, a flash burning die, the upper electrode and the lower electrode; the flash system provides a flash loop for the flash sample;
the induction heating system is used for heating and insulating a flash burning sample; the induction heating system is arranged in the furnace body;
the cooling system is used for cooling the furnace body;
and the vacuum system is used for vacuumizing the interior of the furnace body.
Further, the pressure head and the electrode are fixedly connected by threads, or the electrode is directly nested and fixed in a hole in the center of the end part of the pressure head;
a pressure frame is arranged outside the furnace body, the top end of an upper pressure head is contacted with the lower plane of an upper electrode plate to lead the upper electrode out of the furnace body, and a glass fiber plate or a polytetrafluoroethylene plate is adopted for insulation between the upper plane of the upper electrode plate and a pressure sensor fixed on the pressure frame;
the movable lower pressure head is driven by a servo electric cylinder, the bottom end of the movable lower pressure head is contacted with the upper plane of the lower electrode plate to lead the lower electrode out of the furnace body, and the lower electrode plate is insulated from the servo electric cylinder by adopting a glass fiber plate or a polytetrafluoroethylene plate; dynamic seal (such as oil seal) is adopted between the lower pressure head and the furnace body.
Furthermore, the upper pressure head and the lower pressure head are water-cooled and are insulated from the furnace body by adopting a glass fiber plate or a polytetrafluoroethylene material with certain mechanical property.
Furthermore, the servo electric cylinder (0-20T) is adjustable in pressurization, pressure relief and displacement control rate, and a constant pressure mode and a user-defined pressure mode (a settable loading curve) can be selected.
Furthermore, the furnace body is a horizontal cylinder, and the wall of the cylinder is of a water-cooling double-layer stainless steel structure.
Furthermore, the furnace body is correspondingly provided with a front door and a rear door, the front door is provided with an observation window or a radiation temperature measurement window, and the rear door is provided with a thermocouple, a vacuum extraction opening and a vacuum measurement device.
Further, as one of the innovation points of the invention, the flash burning mould is in a hollow cylindrical shape and has a 3-layer structure, and a flash burning sample is placed in the hollow part; the outermost layer of the flash burning die is a high-temperature-resistant heat-insulating material and is used for reducing the temperature gradient inside the flash burning die, the secondary outer layer is a high-temperature-resistant metal-based material (used under the condition of high flash burning pressure) and also is high-strength graphite (used under the condition of low flash burning pressure), the secondary outer layer is used for bearing the flash burning pressure (the pressure bearing of the inner layer is not influenced even if the innermost layer is broken) and can be used as a heating body by induction heating, so that a flash burning sample is conducted and heated to reach the flash burning temperature, the secondary outer layer material is flexibly selected, the flash burning pressure of 2GPa can be applied, and the flash burning temperature of 1500 ℃ can be provided; the innermost layer is made of a high-temperature-resistant insulating material and is used for electrically insulating the flash burning sample from the secondary outer layer at the flash burning temperature (even if the innermost layer is broken, the electrical insulation between the flash burning sample and the secondary outer layer is not influenced), and the current of a flash burning power supply is ensured to completely pass through the flash burning sample, so that the flash burning purpose is achieved; the mould of dodging burns is supported by high temperature resistant mould seat for reduce the heat conduction effect of dodging the fever mould and lower pressure head, go up the pressure head and dodge the fever in-process and not contact with the mould of dodging, avoid the electric current to pass through the mould of dodging to burn.
Furthermore, the maximum size of the diameter of the flash-burned sample can reach 30mm, and the height depends on the parameters of a flash-burned power supply.
Further, the outermost layer of the flash firing mould is made of porous mullite or carbon felt; the secondary outer layer is made of high-speed steel, hard alloy or high-strength graphite; the innermost layer is made of alumina or boron nitride ceramics.
Furthermore, as one of the innovative points of the present invention, the flash power supply can be selected according to the electrical properties of the flash material to initiate thermal runaway to the maximum extent, so as to implement flash combustion, for example, a low-voltage and large-current pulse power supply is selected for a metal material with good room temperature conductivity; the preheated oxide ceramic material with certain conductivity selects a direct current constant current power supply with high voltage and low current. The flash power supply is connected with the upper electrode plate and the lower electrode plate through leads to form a flash loop.
Further, the induction heating system comprises an induction heating power supply (for example, parameters are 10-30 kW and 15-80 kHz) and an induction heating coil, and the induction heating system is used for heating the induction heating power supplyThe heating coil is fixed on the furnace body through an insulating column and is connected with the water-cooled cable through a motor leading-out device; the flash burning sample, the flash burning die and the induction heating coil are arranged with the same axial lead, so that the flash burning current is parallel to the magnetic induction line direction of the induction coil, the current path is prevented from being interfered, and the size of the induction heating constant temperature area is, for example, the
Figure BDA0002600988800000041
Furthermore, the cooling system adopts a water cooling system, the water cooling system is composed of various pipeline valves and other related devices, and the water cooling system has the function of automatically cutting off a power supply by sound and light alarm when water is cut off.
Furthermore, the vacuum system consists of an oil rotary vane pump, an electromagnetic control valve (preventing the oil from being pumped back by a mechanical pump due to sudden power failure), a vacuum gauge, a vacuum pipeline and a vacuum valve, the pumping speed is 240L/min, and the working vacuum degree is less than or equal to 50Pa (change according to material deflation); the furnace body is kept in a vacuum state or filled with protective atmosphere after being pre-vacuumized.
Furthermore, the upper pressure head and the lower pressure head are made of high-strength graphite blocks or hard alloys, have the diameter of 80-100 mm, are used for applying pressure and are used as conductors for connecting a flash burning loop.
Furthermore, as one of the innovation points of the invention, the material of the upper electrode and the lower electrode is a composite electrode composed of one or any two of magnetic steel, graphite, high-speed steel, hard alloy, copper-based alloy, molybdenum-based alloy and tungsten-based alloy, and the electrode is connected with a pressure head to transmit pressure to the flash burning sample to realize pressure assistance and simultaneously serve as a conductor for connecting the flash burning sample into a flash burning loop; the contact areas of the upper electrode, the lower electrode and the flash burning sample are positioned in the center of the induction coil, the end areas of the upper electrode and the lower electrode which are in contact with the flash burning sample are heated by induction, and the electrode can be independently used as a heating body for conducting heating of the flash burning sample under the condition that a secondary outer layer is not used as the heating body; the composite electrode is formed by stacking metal materials with magnetism (such as magnetic steel and partial high-speed steel) and high-temperature-resistant high-strength metal base materials (such as partial high-speed steel, hard alloy, molybdenum-based alloy and tungsten-based alloy), wherein the metal materials with magnetism are used for providing efficient induction heating for a contact area of the electrode and a flash burning sample, and the high-temperature-resistant high-strength metal base materials are used for bearing higher flash burning pressure.
Furthermore, the device also comprises a control system, wherein the control system adopts a combination of a PLC and a high-precision digital instrument, a true color touch screen is used as a human-computer interaction interface, an operation button is integrated, control instructions and process parameters reach a PCL controller and a temperature control meter, various process information (such as temperature, pressure, displacement, equipment working state and the like) is displayed and recorded, and manual and automatic control can be realized.
The invention has the beneficial effects that: the method not only overcomes the inherent defects in the traditional flash sintering technology, but also integrates the functions of the flash discharge plasma sintering equipment, and can realize most flash sintering processes proposed by domestic and foreign scholars in a simpler and more compact configuration. Meanwhile, a flash power supply can be flexibly selected according to the electrical properties of the flash sintered material to trigger thermal runaway, so that the maximum densification level and the fine regulation and control of the microstructure of a sample are realized, and the method has universality on metal and ceramic materials. And the pressure-assisted flash sintering belongs to one of the latest research directions in the flash sintering academic community and the technical community at present, and is expected to further reduce the flash sintering temperature and the densification time. The invention can easily realize the pressure assistance in the flash combustion process and provide a new preparation means for the research field. In addition, the invention has great application potential in the nuclear fuel industry.
Drawings
Fig. 1 is a schematic structural diagram of a pressure-assisted induction heating vacuum-atmosphere flash sintering apparatus according to an embodiment of the present invention.
FIG. 2 is a schematic view showing the connection between the furnace body and the systems in the embodiment.
Fig. 3 is a schematic view of a flash mold.
FIG. 4 is a schematic view of a composite electrode according to an embodiment.
FIG. 5 is a schematic view of the appearance of the samples of examples 1, 2, 3 and 4 and their SEM pictures; wherein (a) example 1; (b) example 2; (c) example 3; (d) example 4.
FIG. 6 is a schematic view of the appearance of the samples of examples 5, 6, 7 and 8 and their SEM pictures; wherein (a) example 5; (b) example 6; (c) example 7; (d) example 8.
FIG. 7 is a photograph showing the appearance of the samples of examples 9, 10, 11 and 12 and their SEM pictures; wherein (a) example 9; (b) example 10; (c) example 11; (d) example 12.
Wherein: 1-a pressure sensor; 2-an upper insulating plate; 3-an upper electrode plate; 4-a pressure frame; 5-a wire; 6-flash power supply; 7-flash firing the mould; 8- (movable) lower ram; 9-a lower insulating plate; 10-servo electric cylinder; 11-a lower electrode plate; 12-high temperature resistant die holder; 13-a lower electrode; 14-flash-burning the sample; 15-induction heating power supply; 16-an induction heating coil; 17-an upper electrode; 18-furnace body; 19-an upper pressure head; 20-a rear door; 21-gauge tube seat; 22-a thermocouple; 23-vacuum pump connection base; 24-front door; 25-observation window (radiation temperature measurement window); 26- (flash mold) outermost layer; 27- (flash mold) minor outer layer; 28- (flash mold) innermost layer; 29-high temperature resistant high strength metal based material; 30-magnetic metal material.
Detailed Description
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be noted that technical features or combinations of technical features described in the following embodiments should not be considered as being isolated, and they may be combined with each other to achieve better technical effects.
As shown in fig. 1, a pressure-assisted induction heating vacuum atmosphere flash sintering apparatus according to an embodiment of the present invention includes a furnace body 18, a pressure system, a flash firing system, an induction heating system, a cooling system, and a vacuum system; the pressure system comprises an upper pressure head 19 which is fixedly arranged relative to the top of the furnace body 18, a movable lower pressure head 8 and a servo electric cylinder 10; the end part of the upper pressure head 19 is provided with an upper electrode 17, and the end part of the lower pressure head 8 is provided with a lower electrode 13; the servo electric cylinder 10 drives the lower pressure head 8 to move; when the upper pressing head 19 and the lower pressing head 8 move relatively, the upper electrode 17 and the lower electrode 13 are driven to provide pressure for the flash burning sample 14; the flash burning system comprises a flash burning power supply 6, a flash burning die 7, the upper electrode 17 and the lower electrode 13; the flash system provides a flash loop for the flash sample 14; the induction heating system is used for heating and insulating the flash-burned sample 14; the induction heating system is arranged in the furnace body 18; the cooling system is used for cooling the furnace body 18; the vacuum system is used for vacuumizing the interior of the furnace body 18.
Preferably, the upper pressure head 19 is fixed on the furnace top, the upper electrode 17 is led out of the furnace body through the upper electrode plate 3 (tungsten copper plate), and the upper electrode plate 3 is insulated from the pressure sensor 1 fixed on the pressure frame 4 by the upper insulating plate 2; the movable lower pressure head 8 leads a lower electrode 13 out of the furnace body through a lower electrode plate 11 and is connected with a servo electric cylinder 10; the movable lower pressure head 8 and the furnace body 18 are in dynamic seal; the lower electrode plate 11 is insulated from the pressure frame 4 and the servo cylinder 10 by the lower insulating plate 9. The flash burning sample 14 and the die 7 are arranged coaxially with the induction coil 16, so that the flash burning current is parallel to the magnetic induction line direction of the induction coil 16, and the current path is prevented from being interfered; the flash mold 7 is supported by a high temperature resistant mold base 12. The induction coil is connected with a water-cooling cable on the induction heating power supply 15 through an electrode lead-out device. The flash power supply 6 is connected with the upper electrode plate 3 and the lower electrode plate 11 through a lead 5 to form a flash loop.
Preferably, as shown in FIG. 2, the double-deck furnace body 18 is provided with a front door 24 and a rear door 20. The front door 24 is provided with an observation window 25 (temperature measurement window), and the rear door 20 is provided with a gauge tube seat 21 (for placing a vacuum measurement gauge tube), a thermocouple 22 (capable of measuring the temperature of any point on a mold or an electrode through contact), and a vacuum pump connecting seat 23.
Preferably, the structure of the flash burning mold 7 is as shown in fig. 3, and is a hollow cylinder shape, and has a 3-layer structure, the flash burning sample 14 is placed in the hollow part, and the outermost layer 26 is a high temperature resistant heat insulating material (such as porous mullite or carbon felt, etc.) for reducing the temperature gradient inside the flash burning mold; the secondary outer layer 27 is made of a high-temperature-resistant metal-based material or graphite, such as high-speed steel, hard alloy and the like (used under the condition of high flash pressure) and high-strength graphite and the like (used under the condition of low flash pressure), the secondary outer layer 27 is used for bearing the flash pressure (even if the innermost layer 28 is broken, the bearing of the innermost layer is not influenced), and the secondary outer layer 27 can be used as a heating body by induction heating, so that a flash sample is conducted and heated to reach the flash temperature, the secondary outer layer 27 material is flexibly selected, the flash pressure of 2GPa can be applied, and the flash temperature of 1500 ℃ can be provided; the innermost layer 28 is made of a high-temperature-resistant insulating material (such as alumina, boron nitride ceramic and the like) and is used for electrically insulating the flash-burned sample 14 and the secondary outer layer 27 at the flash-burning temperature (even if the innermost layer 28 is broken, the electrical insulation between the flash-burned sample 14 and the secondary outer layer 27 is not affected), and the current of a flash-burning power supply is ensured to completely pass through the flash-burned sample 14, so that the flash-burning purpose is achieved; dodge and burn mould 7 and support by high temperature resistant die holder 12 for reduce to dodge and burn mould 7 and the heat conduction effect of pressure head 8 down, go up pressure head 19 and dodge and burn the in-process and not contact with dodging and burn mould 7, avoid the electric current through dodging and burn mould 7. The diameter of the flash-burned sample 14 can reach 30mm at the maximum size, and the height depends on the parameters of the flash-burned power supply 6. The electrodes 13 and 17 may be single-structure integral electrodes containing only one material, or composite-structure electrodes as shown in fig. 4 may be formed by stacking high-temperature-resistant high-strength metal-based materials 29 (part of high-speed steel, cemented carbide, molybdenum-based alloy, and tungsten-based alloy) and magnetic metal materials 30 (part of high-speed steel and magnetic steel), wherein the magnetic metal materials 30 are used for providing efficient induction heating of the contact area between the electrodes and the sample, and the high-temperature-resistant high-strength metal-based materials 29 are used for bearing higher flash firing pressure.
Preferably, the flash firing mold 7 has a structure as shown in fig. 3, and the outermost layer 26 is a high temperature resistant heat insulating material (such as porous mullite or carbon felt); the secondary outer layer 27 is made of a high-temperature-resistant metal-based material or graphite, such as high-speed steel, hard alloy and the like (used under a condition of high bearing pressure) and high-strength graphite and the like (used under a condition of low bearing pressure and used as a heating barrel to provide a preheating temperature of 800-1500 ℃; the innermost layer 28 is a high temperature resistant insulating material (e.g., alumina, boron nitride ceramic, etc.). The maximum size of the diameter of the flash-burned sample can reach 30mm, and the height of the flash-burned sample is determined according to parameters of a flash-burned power supply. The electrodes 13, 17 may be single-structure monolithic electrodes comprising only one material, or may be composite-structure electrodes as shown in fig. 4, and are composed of a high-temperature strength metal-based material 29 (such as pure tungsten, high-speed steel, cemented carbide, etc.) and a magnetic metal material 30 (such as carbon steel, etc.). The composite structure electrode can better concentrate induction heating energy and has better high-temperature bearing capacity.
Example 1
This example is a pressure assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature is set to 770 ℃, the pressure is 26MPa, and the diameter of the sample is 6.4 mm. The flash power supply adopts a low-power pulse direct current power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128 mus. In this embodiment, the flash current is set to 0A (i.e. the flash power supply is not turned on), the temperature is maintained at the preheating temperature and the constant pressure for 30s, the appearance photograph and the microstructure of the sample are shown in fig. 5 (a), the density is 71.1%, and the grain size is 130.1 nm.
Example 2
This example is a pressure assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature is set to 770 ℃, the pressure is 26MPa, and the diameter of the sample is 6.4 mm. The flash power supply adopts a low-power pulse direct current power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128 mus. In this example, the flash current was set to 50A, the power supply was turned on at the preheating temperature and the constant pressure, and the power supply was turned off immediately after 30 seconds, and the photograph of the appearance and the microstructure of the sample were as shown in fig. 5 (b), and the density was 77.3% and the grain size was 200.7 nm.
Example 3
This example is a pressure assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature is set to 770 ℃, the pressure is 26MPa, and the diameter of the sample is 6.4 mm. The flash power supply adopts a low-power pulse direct current power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128 mus. In this example, the flash current was set to 100A, the power was turned on at the preheating temperature and the constant pressure, and the power was turned off immediately after 30 seconds, and the photograph of the appearance and the microstructure of the sample were as shown in fig. 5 (c), and the density and the grain size were 91.9% and 687.5nm, respectively.
Example 4
This example is a pressure assisted flash sintering of commercial ZnO powder. The induction heating preheating temperature is set to 770 ℃, the pressure is 26MPa, and the diameter of the sample is 6.4 mm. The flash power supply adopts a low-power pulse direct current power supply, the initial electric field intensity is about 80V/cm, the frequency is 1000Hz, and the pulse width is 128 mus. In this example, the flash current was set to 150A, the power supply was turned on at the preheating temperature and the constant pressure, and the power supply was turned off immediately after 30 seconds, and the appearance photograph and the microstructure of the sample were as shown in fig. 5 (d), and the density was 95.2% and the grain size was 912.4 nm.
Example 5
Due to nuclear fuel, e.g. uranium dioxide (UO)2) And the like in the laboratory, the present example uses commercial nano-CeO2The powder was used to simulate pressure assisted flash sintering preparation of nanostructured uranium dioxide fuel pellets. The induction heating preheating temperature is set to 750 ℃, the pressure is 810MPa, and the diameter of the sample is 6.0 mm. The flash power supply adopts a low-power direct current constant current power supply, and the initial electric field intensity is about 500V/cm. In this embodiment, the flash current is set to 0A (i.e., the flash power supply is not turned on), the temperature is maintained at the preheating temperature and the constant pressure for 3min, the appearance photograph and the microstructure of the sample are shown in fig. 6 (a), the density is 91.2%, and the grain size is smaller than 100 nm.
Example 6
Due to nuclear fuel, e.g. uranium dioxide (UO)2) And the like in the laboratory, the present example uses commercial nano-CeO2The powder was used to simulate pressure assisted flash sintering preparation of nanostructured uranium dioxide fuel pellets. The induction heating preheating temperature is set to 750 ℃, the pressure is 810MPa, and the diameter of the sample is 6.0 mm. The flash power supply adopts a low-power direct current constant current power supply, and the initial electric field intensity is about 500V/cm. In this embodiment, the flash current is set to 1A, the power supply is turned on at the preheating temperature and under the constant pressure, the power supply is turned off immediately after the current reaches the peak value of 1s, the entire process lasts for about 3min, the appearance photograph and microstructure of the sample are shown in fig. 6 (b), the density is 92.5%, and the grain size is smaller than 100 nm.
Example 7
Due to nuclear fuel, e.g. uranium dioxide (UO)2) And the like in the laboratory, the present example uses commercial nano-CeO2The powder was used to simulate pressure assisted flash sintering preparation of nanostructured uranium dioxide fuel pellets. The induction heating preheating temperature is set to 750 ℃, the pressure is 810MPa, and the diameter of the sample is 6.0 mm. Flash burningThe power supply adopts a low-power direct current constant current power supply, and the initial electric field intensity is about 500V/cm. In this embodiment, the flash current is set to 1A, the power supply is turned on at the preheating temperature and under the constant pressure, the power supply is turned off immediately after the current reaches the peak value of 5s, the entire process lasts for about 3min, the appearance photograph and microstructure of the sample are shown in fig. 6 (c), the density is 94.7%, and the grain size is less than 100 nm.
Example 8
Due to nuclear fuel, e.g. uranium dioxide (UO)2) And the like in the laboratory, the present example uses commercial nano-CeO2The powder was used to simulate pressure assisted flash sintering preparation of nanostructured uranium dioxide fuel pellets. The induction heating preheating temperature is set to 750 ℃, the pressure is 810MPa, and the diameter of the sample is 6.0 mm. The flash power supply adopts a low-power direct current constant current power supply, and the initial electric field intensity is about 500V/cm. In this embodiment, the flash current is set to 1A, the power supply is turned on at the preheating temperature and under the constant pressure, the power supply is turned off immediately after the current reaches the peak value for 10s, the entire process lasts for about 3min, the appearance photograph and microstructure of the sample are shown in fig. 6 (d), the density is 96.5%, and the grain size is less than 100 nm.
Example 9
This example is a pressure assisted flash sintering of commercial atomized Al-12Si powder. The powder has good conductivity at room temperature, so that a high-power pulse direct-current power supply is adopted to forcibly initiate thermal runaway, flash burning is realized, and induction heating preheating is not needed. The pressure was 631MPa, the sample diameter was 10.5mm, the initial electric field strength was about 10V/cm, the frequency was 30kHz, and the pulse width was 100. mu.s. In this example, the flash current was set to 1200A, the power was turned on at room temperature under a constant pressure, and immediately after 1s, the power was turned off, and the appearance photograph and microstructure of the sample were as shown in fig. 7 (a), and the density was 93.0% and the hardness was 66 HV.
Example 10
This example is a pressure assisted flash sintering of commercial atomized Al-12Si powder. The powder has good conductivity at room temperature, so that a high-power pulse direct-current power supply is adopted to forcibly initiate thermal runaway, flash burning is realized, and induction heating preheating is not needed. The pressure was 631MPa, the sample diameter was 10.5mm, the initial electric field strength was about 10V/cm, the frequency was 30kHz, and the pulse width was 100. mu.s. In this example, the flash current was set to 1200A, the power was turned on at room temperature under a constant pressure, and the power was turned off immediately after 10 seconds, and the photograph of the appearance and the microstructure of the sample were as shown in fig. 7 (b), and the density was 97.9% and the hardness was 98 HV.
Example 11
This example is a pressure assisted flash sintering of commercial atomized Al-12Si powder. The powder has good conductivity at room temperature, so that a high-power pulse direct-current power supply is adopted to forcibly initiate thermal runaway, flash burning is realized, and induction heating preheating is not needed. The pressure was 631MPa, the sample diameter was 10.5mm, the initial electric field strength was about 10V/cm, the frequency was 30kHz, and the pulse width was 100. mu.s. In this example, the flash current was set to 1200A, the power was turned on at room temperature and constant pressure, and the power was turned off immediately after 20 seconds, and the photograph of the appearance and the microstructure of the sample were as shown in fig. 7 (c), and the density was 99.8% and the hardness was 81 HV.
Example 12
This example is a pressure assisted flash sintering of commercial atomized Al-12Si powder. The powder has good conductivity at room temperature, so that a high-power pulse direct-current power supply is adopted to forcibly initiate thermal runaway, flash burning is realized, and induction heating preheating is not needed. The pressure was 631MPa, the sample diameter was 10.5mm, the initial electric field strength was about 10V/cm, the frequency was 30kHz, and the pulse width was 100. mu.s. In this example, the flash current was set to 1200A, the power was turned on at room temperature under a constant pressure, and the power was turned off immediately after 30 seconds, and the photograph of the appearance and the microstructure of the sample were as shown in fig. 7 (d), and the density was 98.3% and the hardness was 101 HV.
While several embodiments of the present invention have been presented herein, it will be appreciated by those skilled in the art that changes may be made to the embodiments herein without departing from the spirit of the invention. The above examples are merely illustrative and should not be taken as limiting the scope of the invention.

Claims (11)

1. A pressure-assisted induction heating vacuum atmosphere flash sintering device is characterized by comprising a furnace body, a pressure system, a flash burning system, an induction heating system, a cooling system and a vacuum system;
the pressure system comprises an upper pressure head and a movable lower pressure head, wherein the upper pressure head is fixedly arranged relative to the top of the furnace body; the end part of the upper pressure head is provided with an upper electrode, and the end part of the lower pressure head is provided with a lower electrode; when the upper pressing head and the lower pressing head move relatively, the upper electrode and the lower electrode are driven to provide pressure for flash burning samples;
the flash burning system comprises a flash burning power supply, a flash burning die, the upper electrode and the lower electrode; the flash system provides a flash loop for a flash sample;
the induction heating system is used for heating and insulating a flash burning sample; the induction heating system is arranged in the furnace body;
the cooling system is used for cooling the furnace body;
and the vacuum system is used for vacuumizing the interior of the furnace body.
2. The pressure-assisted induction heating vacuum atmosphere flash sintering apparatus according to claim 1,
the pressure head and the electrode are fixedly connected by threads, or the electrode is directly embedded and fixed in a hole in the center of the end part of the pressure head;
a pressure frame is arranged outside the furnace body, the top end of an upper pressure head is contacted with the lower plane of an upper electrode plate to lead the upper electrode out of the furnace body, and a glass fiber plate or a polytetrafluoroethylene plate is adopted for insulation between the upper plane of the upper electrode plate and a pressure sensor fixed on the pressure frame;
the movable lower pressure head is driven by a servo electric cylinder, the bottom end of the movable lower pressure head is contacted with the upper plane of the lower electrode plate to lead the lower electrode out of the furnace body, and the lower electrode plate is insulated from the servo electric cylinder by adopting a glass fiber plate or a polytetrafluoroethylene plate; the lower pressure head and the furnace body are in dynamic seal.
3. The pressure-assisted induction heating vacuum atmosphere flash sintering device according to claim 1 or 2, wherein the furnace body is a horizontal cylinder, and the wall of the cylinder is of a water-cooled double-layer stainless steel structure.
4. The pressure-assisted induction heating vacuum atmosphere flash sintering device according to claim 3, wherein the furnace body is correspondingly provided with a front door and a rear door, the front door is provided with an observation window or a radiation temperature measurement window, and the rear door is provided with a thermocouple, a vacuum extraction opening and a vacuum measurement device.
5. The pressure-assisted induction heating vacuum atmosphere flash sintering apparatus according to claim 1, wherein the flash mold has a hollow cylindrical shape having a 3-layer structure, and a flash sample is placed in the hollow portion; the outermost layer of the flash burning die is a high-temperature-resistant heat-insulating material, the secondary outer layer is a high-temperature-resistant metal-based material or graphite, and the innermost layer is a high-temperature-resistant insulating material; the flash burning die is supported by the high-temperature resistant die seat.
6. The pressure-assisted induction heating vacuum atmosphere flash sintering device according to claim 5, wherein the outermost layer material of the flash firing mold is porous mullite or carbon felt; the secondary outer layer is made of high-speed steel, hard alloy or high-strength graphite; the innermost layer is made of alumina or boron nitride ceramics.
7. The pressure-assisted induction heating vacuum atmosphere flash sintering device according to claim 5, wherein the induction heating system comprises an induction heating power supply and an induction heating coil, the induction heating coil being fixed to the furnace body by an insulating column; the flash burning sample, the flash burning die and the induction heating coil are arranged with the same axial lead, so that the flash burning current is parallel to the direction of the magnetic induction line of the induction coil.
8. The pressure-assisted induction heating vacuum atmosphere flash sintering device according to claim 1, wherein the vacuum system comprises a rotary vane pump, an electromagnetic control valve, a vacuum gauge, a vacuum pipeline and a vacuum valve, the pumping speed is 240L/min, and the working vacuum degree is less than or equal to 50 Pa; the furnace body is kept in a vacuum state or filled with protective atmosphere after being pre-vacuumized.
9. The pressure-assisted induction heating vacuum atmosphere flash sintering device according to claim 1, wherein the upper ram and the lower ram are made of high-strength graphite blocks or hard alloys, and have a diameter of 80-100 mm; the upper electrode and the lower electrode are composite electrodes formed by one or any two of magnetic steel, graphite, high-speed steel, hard alloy, copper-based alloy, molybdenum-based alloy and tungsten-based alloy.
10. The pressure-assisted induction heating vacuum atmosphere flash sintering apparatus of claim 1, used for flash sintering preparation of ion conductor ceramics, semiconductor ceramics, electronic conductor ceramics, insulator ceramics, metals and metal matrix composites.
11. The pressure-assisted induction heating vacuum atmosphere flash sintering device of claim 1, which is used for flash sintering preparation of a plurality of nuclear fuel pellets, wherein materials of the plurality of nuclear fuel pellets comprise uranium dioxide, uranium carbide, uranium nitride, uranium silicide, and composite materials taking uranium dioxide, uranium carbide, uranium nitride and uranium silicide as matrixes.
CN202010723873.0A 2020-07-24 2020-07-24 Pressure-assisted induction heating vacuum atmosphere flash sintering device Pending CN111981847A (en)

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CN113831144A (en) * 2021-10-26 2021-12-24 中国工程物理研究院材料研究所 Method for preparing ceramic material by multi-field coupling ultra-fast sintering
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CN112390629A (en) * 2020-12-04 2021-02-23 吉林大学 Device and method for rapidly sintering ceramic
CN113154882A (en) * 2021-04-27 2021-07-23 华南师范大学 Non-pressure rapid sintering device and method for 3D printing
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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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CN114058798A (en) * 2021-11-26 2022-02-18 上海大学 Flash annealing process and device for La-Fe-Si series alloy
WO2023154289A1 (en) * 2022-02-09 2023-08-17 The Regents Of The University Of Colorado, A Body Corporate Flash sintering with electrical and magnetic fields
CN115304369A (en) * 2022-03-09 2022-11-08 陕西科技大学 Preparation method of high-dielectric high-breakdown strontium titanate ceramic
CN115304369B (en) * 2022-03-09 2023-08-22 陕西科技大学 Preparation method of high-dielectric high-breakdown strontium titanate ceramic
CN115502401A (en) * 2022-08-29 2022-12-23 合肥工业大学 Auxiliary sintering device for powder metallurgy field with coupled heating
CN116379767A (en) * 2022-12-26 2023-07-04 无锡海古德新技术有限公司 Three-dimensional hot-pressing vibration sintering furnace
CN116379767B (en) * 2022-12-26 2023-10-10 无锡海古德新技术有限公司 Three-dimensional hot-pressing oscillation sintering furnace

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