CN108947542B - Direct flash-firing forming preparation method of ceramic powder raw material - Google Patents
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Abstract
The invention relates to a preparation method for directly flash-firing ceramic powder raw materials, which comprises the following steps: (1) pouring the raw materials into a mould, and vibrating to flatten the surface of the raw materials; (2) putting the die into a flash firing device for directly molding the ceramic powder raw material, and applying 40-50 MPa pressure to enable the ceramic powder raw material to be in the middle of a heating area; (3) turning on an auxiliary heating power supply (an induction heating power supply here), and heating to 900-1000 ℃ at a speed of 100-110 ℃/min or until a flash phenomenon occurs; (4) turning on a high-voltage direct-current flash power supply, and applying direct current to two sides of the sample to linearly increase the voltage by about 200V/cm until a flash phenomenon occurs; (5) controlling the current to be reduced to below 1000A, and keeping the current constant; lasting for 20-50 s; (6) cooling to room temperature to obtain a compact sintered body; (7) and grinding and polishing the sintered body to obtain the required product.
Description
Technical Field
The invention relates to the technical field of ceramic sintering forming technology and equipment used by the same, in particular to a preparation method for directly flash-firing and forming ceramic powder raw materials.
Background
The ceramic material is an important industrial material, and different ceramics have different mechanical, electrical, optical, acoustic, magnetic and other properties, so that the ceramic material has various applications and becomes an indispensable important material in the modern society.
The preparation process of the ceramic material is various, and the process flow of molding, sintering and machining is generally adopted. Sintering is the most important process in the ceramic material preparation process, and is an important link for the material performance. In the conventional high temperature sintering process, it requires a large amount of energy consumption, which may cause serious environmental problems. In order to save energy and protect the environment, many new sintering techniques have been developed, such as microwave sintering, hot isostatic pressing sintering, spark plasma sintering, etc.
The new technologies are applied in different fields, and make important contribution to the development of ceramic materials. In 2010 Rishi Raj proposed a new ceramic sintering method, flash firing method. The flash firing technology can realize the densification process of the ceramic within a few seconds, and simultaneously greatly reduces the sintering temperature, thereby having the advantages of high efficiency and low energy consumption. On this basis, many researchers have proposed various sintering apparatuses based on the flash firing principle.
For example, patent CN 206089473U describes an electric field assisted ceramic low-temperature fast firing device using a flat heater metal electrode, which has the advantages of working in air atmosphere and easy measurement and control of the sintering process. CN 107202495 a proposes a flash firing structure using a metal electrode of a hydraulic press, which can be used for flash firing sintering of pressed green bodies.
However, the conventional sintering equipment can only be used for preparing rough blanks and green blanks, and cannot prepare compact sintered bodies.
Therefore, it is necessary to provide a method for preparing ceramic powder by direct flash firing to solve the above problems.
Disclosure of Invention
The invention aims to provide a direct flash firing forming preparation method of a ceramic powder raw material, which is a design scheme of direct flash firing equipment using ceramic powder as a raw material and does not need to prepare a ceramic green body by using a dry pressing, cold isostatic pressing or tape casting method in advance, so that the production flow of ceramic products is greatly simplified, and the shape and the size of the product can be more accurately controlled by using high-temperature ceramic and graphite as mould materials, so that the flash firing technology has the basis of industrial application.
The technical scheme is as follows:
a method for preparing ceramic powder by directly flash firing raw materials comprises the following steps:
(1) pouring the raw materials into a mould, and vibrating to flatten the surface of the raw materials;
(2) putting the die into a flash firing device for directly molding the ceramic powder raw material, and applying 40-50 MPa pressure to enable the ceramic powder raw material to be in the middle of a heating area;
(3) turning on an auxiliary heating power supply (an induction heating power supply here), and heating to 900-1000 ℃ at a speed of 100-110 ℃/min or until a flash phenomenon occurs;
(4) turning on a high-voltage direct-current flash power supply, and applying direct current to two sides of the sample to linearly increase the voltage by about 200V/cm until a flash phenomenon occurs;
(5) controlling the current to be reduced to below 1000A, and keeping the current constant; lasting for 20-50 s;
(6) cooling to room temperature to obtain a compact sintered body;
(7) and grinding and polishing the sintered body to obtain the required product.
Further, in the step (1), the raw material is composite zirconia granulated powder or mixed rare earth oxide granulated powder.
Furthermore, the mixed rare earth oxide granulation powder is formed by mixing lutetium oxide, gadolinium oxide and europium oxide, wherein the lutetium oxide content is 70-90 mol%, the gadolinium oxide content is 10-20 mol%, and the europium oxide content is 0-10 mol%.
Furthermore, the component of the composite zirconia granulated powder is yttria-stabilized zirconia, wherein the content of yttria is 3-12 mol%, and the content of alumina is 0-66 mol%.
Further, the direct ceramic powder raw material forming flash burning equipment comprises a pressurizing device, a vacuum chamber, an auxiliary heating power supply, a high-voltage direct current flash burning power supply, a control system and a cooling system; the raw materials are placed in a mould consisting of high-temperature ceramic and graphite, positioned in the center of the interior of a vacuum chamber and constrained by the pressure of a pressurization system; the auxiliary heating power supply enters the vacuum chamber through the outer wall of the vacuum chamber to heat the ceramic powder raw material; the high-voltage direct-current flash combustion power supply applies voltage to the graphite mould through water-cooled copper electrodes at the upper pressure head and the lower pressure head of the pressurizing device;
when the ceramic powder sintering device is used, the heating body of the auxiliary heating system is used for providing the preheating temperature required by the ceramic powder raw material before flash sintering, and meanwhile, a certain pressure is applied through the pressurizing device; when the temperature reaches a set value, a high-voltage direct-current flash power supply applies a direct-current electric field to form flash combustion, so that low-temperature rapid densification of the ceramic material is realized; the high-voltage direct-current flash combustion power supply can be controlled by a program, the voltage control is switched into the current control when flash combustion occurs, heating is finished after a certain time is continued, and then the high-voltage direct-current flash combustion power supply is cooled to room temperature.
Furthermore, a temperature detection device for measuring the temperature of the sample is arranged near the die in the vacuum chamber, and the temperature detection device can select a thermocouple when the temperature is lower than 1600 ℃; the temperature data input control system is used for controlling current and voltage parameters of the auxiliary heating power supply and the flash power supply; so that the sample can realize stable heating sintering.
Furthermore, when the temperature is higher than 1600 ℃, an infrared thermometer can be used for replacing a thermocouple to realize temperature measurement.
Compared with the prior art, the direct flash firing equipment using the ceramic powder as the raw material has the advantages that the ceramic green body is prepared without using a dry pressing, cold isostatic pressing or tape casting method in advance, so that the production flow of the ceramic product is greatly simplified, and the shape and the size of the product can be more accurately controlled by using the high-temperature ceramic and the graphite as the die materials, so that the flash firing technology has the basis of industrial application.
Drawings
Fig. 1 is a schematic structural view of the present invention.
Detailed Description
Example 1:
referring to fig. 1, this embodiment shows a flash firing apparatus for directly forming ceramic powder raw material, which includes a pressurizing device 1, a vacuum chamber 3, an auxiliary heating power supply 6, a high voltage dc flash firing power supply 4, a control system 5, and a cooling system 7.
The sample powder is placed in a mould composed of high-temperature ceramic and graphite, is positioned in the center of the interior of a vacuum chamber, and is constrained by the pressure of a pressurization system.
The auxiliary heating power supply enters the vacuum chamber through the outer wall of the vacuum chamber to heat the ceramic powder raw material.
The high-voltage direct-current flash power supply applies voltage to the graphite die through water-cooled copper electrodes at the upper pressure head and the lower pressure head of the pressurizing device.
When the ceramic powder sintering device is used, the heating body of the auxiliary heating system is used for providing the preheating temperature required by the ceramic powder raw material before flash sintering, and meanwhile, a certain pressure is applied through the pressurizing device; when the temperature reaches a set value, a direct current electric field is applied by the high-voltage direct current flash power supply 4 to form flash combustion, so that low-temperature rapid densification of the ceramic material is realized; the high-voltage direct-current flash combustion power supply 4 can be controlled by a program, the voltage control is switched into the current control when flash combustion occurs, heating is finished after a certain time is continued, and then the high-voltage direct-current flash combustion power supply is cooled to room temperature.
And a temperature detection device for measuring the temperature of the sample is arranged near the die in the vacuum chamber 3, and when the temperature is lower than 1600 ℃, the temperature detection device can select a thermocouple, and temperature data is input into the control system and is used for controlling current and voltage parameters of the auxiliary heating power supply and the flash power supply. So that the sample can realize stable heating sintering.
When the temperature is higher than 1600 ℃, an infrared thermometer can be used for replacing a thermocouple to realize temperature measurement.
Wherein: the ceramic powder raw material direct forming flash combustion equipment of this embodiment can make up vacuum system, pressure system, auxiliary heating system and high voltage direct current flash combustion power supply system and observe and control and cooling system thereof:
(1) a vacuum system: as the upper and lower pressure heads (with the function of electrodes) of the die are made of graphite materials, and the graphite in a high-temperature state can be oxidized in the air, the heating part of the device needs to be kept in vacuum or inert gas protection. A set of vacuum chamber is designed in the center of the device, heat shielding materials are configured, and connecting flanges are designed on the upper portion, the lower portion and the periphery of the vacuum chamber and used for connecting an electrode, a water cooling pipeline and a press pressure head. The vacuum chamber is pumped by a vacuum pump through a pipeline, and the cold state ultimate vacuum reaches below 10 Pa. Meanwhile, an inflation device is designed, nitrogen can be filled in for protection of inert gas, and hydrogen can be filled in to form reducing atmosphere.
(2) A pressure system:
hydraulic, electric, mechanical or electrohydraulic servo presses may be used as the pressure system. The rated pressure can be selected from 1 to 250 tons. The dwell time is more than ten minutes. The upper pressure head of the press is connected into a vacuum chamber through a sealing corrugated pipe flange or other dynamic sealing modes, is insulated from an electrode through a 99 alumina ceramic wafer, is connected with a water-cooling copper electrode in a downward mode, and forms a pressure system together with a graphite mould.
The graphite mould is made of high-purity hot isostatic pressure graphite through mechanical processing and is divided into an upper mould and a lower mould, and the outer mould is made of insulating ceramic alumina, boron nitride or silicon carbide. The inner cavity is designed to be phi 12-180 mm, and the surface is polished.
(3) Heating system
The heating system is composed of a resistance heating or induction heating power supply and is connected to the vacuum chamber through a flange. The heating body is combined with a heat insulation material to wrap the high-temperature ceramic female die. With a thermocouple inserted in the middle for temperature measurement and control. The power is about 10-200 kilowatts. The working temperature is 400-1000 ℃.
(4) Power supply system
Firstly, a program-controlled direct-current power supply is selected to carry out electric field control, the power supply is connected into a vacuum chamber through an electrode flange, is connected to water-cooled copper electrodes designed on an upper pressure head and a lower pressure head and is connected with a graphite electrode, and therefore a high-voltage direct-current electric field passing through ceramic powder is constructed.
(5) In addition, the device also comprises accessories such as a cabinet, a control platform, a water cooling machine and the like, and is used for ensuring that the system can operate safely and efficiently.
Example 2:
the sintering of the flat zirconia ceramics was carried out using the ceramic powder raw material direct molding flash firing equipment shown in example 1, with the following steps:
(1) pouring the composite zirconia granulation powder into a mold, and vibrating to flatten the surface of the composite zirconia granulation powder;
(2) putting the die into the equipment of the invention, and applying 50MPa pressure to ensure that the ceramic powder raw material is positioned in the middle of the heating area;
(3) turning on an auxiliary heating power supply (induction heating power supply here), and heating to 1000 deg.C at a speed of 100 deg.C/min;
(4) turning on a high-voltage direct-current flash power supply, applying direct current on two sides of the sample, linearly increasing the voltage by about 100V/cm until flash occurs, and rapidly switching to current control at 100mA/mm2Sintering for 2min by current, and cooling to room temperature to obtain a compact sintered body.
The component of the composite zirconia granulated powder in the step (1) is yttria-stabilized zirconia, wherein the content of yttria is 3-12 mol%, and the content of alumina is 0-66 mol%.
The density of the zirconia ceramic sintered body prepared by the embodiment is measured by an Archimedes method, the average density can reach 99.5 percent of the theoretical density, the density is free of micro-cavity defects, the density is measured by a three-point bending method, the bending strength is more than 850 MPa, and the fracture toughness is more than 7 Mpa.m by an indentation method1/2The average grain size is less than 1 micron observed by a scanning electron microscope, and the mechanical property of the product is equivalent to that of a product obtained by a high-temperature sintering technology; the process combines solid phase sintering and flash sintering, the solid phase sintering temperature is 400 ℃ lower than that of hot pressing sintering technology, the total sintering time is not more than 20 minutes, and the process has the advantages of high sintering efficiency, low cost and the likeControllable process, high preparation efficiency and energy conservation, and is suitable for industrial production.
Example 3:
sintering of rare earth oxide transparent ceramic scintillators was carried out using the ceramic powder feedstock direct-fired flash firing equipment demonstrated in example 1, with the following steps:
(1) pouring the mixed rare earth oxide granulation powder (the components are lutetium oxide, gadolinium oxide and europium oxide, wherein the content of lutetium oxide is 70-90 mol%, the content of gadolinium oxide is 10-20 mol%, and the content of europium oxide is 0-10 mol%) into a mold, and oscillating to be flat;
(2) putting the die into the equipment, and applying 40MPa pressure to enable the ceramic powder raw material to be positioned in the middle of a heating area;
(3) turning on an auxiliary heating power supply (induction heating power supply here), and heating to 900 deg.C at a speed of 100 deg.C/min;
(4) turning on a high-voltage direct-current flash power supply, and applying direct current to two sides of the sample to linearly increase the voltage by about 200V/cm until a flash phenomenon occurs;
(5) controlling the current to be reduced to below 1000A, and keeping the current constant; lasting for 20-50 s;
(6) cooling to room temperature to obtain a dense sintered body of the rare earth oxide transparent ceramic scintillator;
(7) and grinding and polishing the sintered body to form the transparent ceramic scintillator product.
The embodiment can provide the transparent ceramic scintillator meeting the application of high-energy X-ray radiation detection, and has the advantages of high preparation speed, high transparency and low cost.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (7)
1. A preparation method for directly flash-firing ceramic powder raw materials is characterized by comprising the following steps:
the method comprises the following steps:
(1) pouring the raw materials into a mould, and vibrating to flatten the surface of the raw materials;
(2) putting the die into a flash firing device for directly molding the ceramic powder raw material, and applying 40-50 MPa pressure to enable the ceramic powder raw material to be in the middle of a heating area;
(3) opening an auxiliary heating power supply, wherein the auxiliary heating power supply is an induction heating power supply, and heating to 900-1000 ℃ at a speed of 100-110 ℃/min;
(4) turning on a high-voltage direct-current flash power supply, and applying direct current to two sides of the sample to linearly increase the voltage by 200V/cm until a flash phenomenon occurs;
(5) controlling the current to be reduced to below 1000A, and keeping the current constant; lasting for 20-50 s;
(6) cooling to room temperature to obtain a compact sintered body;
(7) and grinding and polishing the sintered body to obtain the required product.
2. The direct flash firing forming preparation method of ceramic powder raw material as claimed in claim 1, characterized in that: in the step (1), the raw material is composite zirconia granulated powder or mixed rare earth oxide granulated powder.
3. The direct flash firing forming preparation method of ceramic powder raw material as claimed in claim 2, characterized in that: the mixed rare earth oxide granulation powder is formed by mixing lutetium oxide, gadolinium oxide and europium oxide, wherein the lutetium oxide content is 70-90 mol%, the gadolinium oxide content is 10-20 mol%, and the europium oxide content is 0-10 mol%.
4. The direct flash firing forming preparation method of ceramic powder raw material as claimed in claim 2, characterized in that: the component of the composite zirconia granulated powder is yttria-stabilized zirconia, wherein the content of yttria is 3-12 mol%, and the content of alumina is 0-66 mol%.
5. The direct flash firing forming preparation method of ceramic powder raw material as claimed in claim 3 or 4, characterized in that: the direct forming flash burning equipment for the ceramic powder raw material comprises a pressurizing device, a vacuum chamber, an auxiliary heating power supply, a high-voltage direct current flash burning power supply, a control system and a cooling system; the raw materials are placed in a mould consisting of high-temperature ceramic and graphite, positioned in the center of the interior of a vacuum chamber and constrained by the pressure of a pressurization system; the auxiliary heating power supply enters the vacuum chamber through the outer wall of the vacuum chamber to heat the ceramic powder raw material; the high-voltage direct-current flash combustion power supply applies voltage to the graphite mould through water-cooled copper electrodes at the upper pressure head and the lower pressure head of the pressurizing device; when the ceramic powder sintering device is used, the heating body of the auxiliary heating system is used for providing the preheating temperature required by the ceramic powder raw material before flash sintering, and meanwhile, a certain pressure is applied through the pressurizing device; when the temperature reaches a set value, a high-voltage direct-current flash power supply applies a direct-current electric field to form flash combustion, so that low-temperature rapid densification of the ceramic material is realized; the high-voltage direct-current flash power supply is controlled by a program, voltage control is switched into current control when flash burning occurs, heating is finished after a certain time is continued, and then the high-voltage direct-current flash power supply is cooled to room temperature.
6. The direct flash firing forming preparation method of ceramic powder raw material as claimed in claim 5, characterized in that: a temperature detection device for measuring the temperature of the sample is arranged near the die in the vacuum chamber, and the temperature detection device selects a thermocouple when the temperature is lower than 1600 ℃; the temperature data input control system is used for controlling current and voltage parameters of the auxiliary heating power supply and the flash power supply; so that the sample can realize stable heating sintering.
7. The direct flash firing forming preparation method of ceramic powder raw material as claimed in claim 6, characterized in that: and when the temperature is higher than 1600 ℃, an infrared thermometer is used for replacing a thermocouple to realize temperature measurement.
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