CN111912227A - Rapid sintering equipment and sintering method for dynamically loading coupled alternating current - Google Patents

Rapid sintering equipment and sintering method for dynamically loading coupled alternating current Download PDF

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Publication number
CN111912227A
CN111912227A CN202010749837.1A CN202010749837A CN111912227A CN 111912227 A CN111912227 A CN 111912227A CN 202010749837 A CN202010749837 A CN 202010749837A CN 111912227 A CN111912227 A CN 111912227A
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sintering
dynamic loading
control system
alternating current
pressure
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CN202010749837.1A
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Chinese (zh)
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谢志鹏
许靖堃
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Tsinghua University
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Tsinghua University
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27BFURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
    • F27B17/00Furnaces of a kind not covered by any preceding group
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D11/00Arrangement of elements for electric heating in or on furnaces
    • F27D11/08Heating by electric discharge, e.g. arc discharge
    • F27D11/10Disposition of electrodes
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00Arrangements of controlling devices
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D21/00Arrangements of monitoring devices; Arrangements of safety devices
    • F27D21/0014Devices for monitoring temperature
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/06Forming or maintaining special atmospheres or vacuum within heating chambers
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D9/00Cooling of furnaces or of charges therein
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D7/00Forming, maintaining, or circulating atmospheres in heating chambers
    • F27D7/06Forming or maintaining special atmospheres or vacuum within heating chambers
    • F27D2007/063Special atmospheres, e.g. high pressure atmospheres
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00Arrangements of controlling devices
    • F27D2019/0006Monitoring the characteristics (composition, quantities, temperature, pressure) of at least one of the gases of the kiln atmosphere and using it as a controlling value
    • F27D2019/0009Monitoring the pressure in an enclosure or kiln zone
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F27FURNACES; KILNS; OVENS; RETORTS
    • F27DDETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
    • F27D19/00Arrangements of controlling devices
    • F27D2019/0028Regulation
    • F27D2019/0034Regulation through control of a heating quantity such as fuel, oxidant or intensity of current
    • F27D2019/0037Quantity of electric current

Abstract

The invention relates to a rapid sintering device for dynamically loading coupled alternating current, which comprises the following components: the furnace comprises a furnace frame, wherein a furnace body is arranged in the furnace frame, and a closed pressure-maintaining cabin is formed in the furnace body; the dynamic loading system comprises a dynamic loading generation part and a dynamic loading control part, wherein the dynamic loading generation part is arranged in the pressure maintaining cabin and is used for heating the sintering material; the output end of the dynamic loading control part is connected with the dynamic loading generating part and is used for outputting the total dynamic loading after coupling to the dynamic loading generating part; the sintering control system is arranged outside the pressure maintaining cabin, and the output end of the sintering control system is connected with the input end of the dynamic loading control part; and the alternating current control system is arranged outside the pressure maintaining cabin, the input end of the alternating current control system is connected with the output end of the sintering control system, and the output end of the alternating current control system is connected with the dynamic loading generation part. The equipment can obviously improve the sintering driving force, inhibit the growth of crystal grains, improve the density of a sintered body and improve the material performance.

Description

Rapid sintering equipment and sintering method for dynamically loading coupled alternating current
Technical Field
The invention relates to a rapid sintering device and a rapid sintering method for dynamically loading coupled alternating current, and belongs to the technical field of sintering.
Background
Sintering is one of the most critical steps in the preparation process of advanced structural and functional materials such as high-performance ceramics. In the conventional pressureless sintering process, the surface curvature of the powder is the only sintering driving force. When the temperature rises, the material to be sintered is subjected to diffusion mass transfer under the action of sintering driving force, the porosity of the system is reduced, the density is increased, and finally a compact block material is obtained. However, in the later stage of sintering, the surface curvature of the crystal grains is reduced, the driving force for further densification is significantly reduced, residual pores cannot be effectively discharged, and even the crystal grains grow abnormally, so that the ceramic materials prepared by the pressureless sintering technology often have higher porosity and larger crystal grain size. In response, researchers have developed hot-press sintering techniques. The hot-pressing sintering can apply static loading to the powder to be sintered while sintering, so that additional sintering driving force is provided. The driving force is far greater than the surface curvature driving force, so that the densification process can be effectively promoted, and the sintering temperature is reduced. Compared with pressureless sintering, the compactness of a hot-pressed sintered sample is generally higher, the grain size is smaller, but the particles are difficult to slide and rearrange under the action of static loading and are easy to generate hard agglomeration, so that the uniformity of the microstructure of a final product is still not ideal. Research shows that if static loading can be improved into dynamic loading with a certain period and amplitude, the discharge of tiny residual air holes at the end of sintering can be remarkably promoted, and the ultrahigh-strength fully-dense ceramic is prepared.
Pressureless sintering and hot-pressed sintering are heated using an external heat source, and therefore the rate of temperature rise is usually not higher than 20 ℃/min. During the slow temperature rise, coarsening of the crystal grains inevitably occurs, thereby reducing the driving force for densification at high temperatures. Discharge plasma sintering (SPS) is a new sintering technology developed in the last three decades, which does not use an external heating source during sintering, but heats a material to be sintered by joule heat generated by passing a pulse direct current through a die. The temperature rise rate of the technology can reach hundreds of degrees centigrade per minute, thereby effectively avoiding the coarsening of crystal grains in the temperature rise stage, shortening the sintering time and improving the sintering efficiency. However, the directionality of the pulsed dc current may cause the microstructure at the positive and negative electrodes of the sample to be inconsistent, affecting the overall performance. If the pulsed dc current could be replaced by an alternating current, inhomogeneities in the sample in the direction of the current could be completely avoided. In addition, static loading is adopted in spark plasma sintering, which is not ideal for eliminating hard agglomeration of nano powder. If a dynamic loading with a certain vibration frequency and vibration pressure intensity is introduced, the complete densification of the sample can be realized while the rapid sintering is carried out. And the alternating current is used without complex rectifying and filtering equipment, so that the manufacturing cost of the sintering furnace can be reduced, and the industrial popularization and application are facilitated.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a rapid sintering apparatus and a rapid sintering method for dynamically loading and coupling alternating current, wherein the apparatus uses alternating current to realize rapid heating, which can significantly shorten the sintering time, and simultaneously uses dynamic loading hot pressing sintering to significantly improve the density of the material to be sintered, reduce the grain size, and enhance the performance of the material in various aspects.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a rapid sintering device for dynamically loading coupled alternating current, which comprises the following components:
the furnace comprises a furnace frame, wherein a furnace body is arranged in the furnace frame, and a closed pressure-maintaining cabin is formed in the furnace body;
the dynamic loading system comprises a dynamic loading generation part and a dynamic loading control part, wherein the dynamic loading generation part is arranged in the pressure maintaining cabin and is used for pressurizing and heating the sintering material; the dynamic loading control part is arranged outside the pressure maintaining cabin, and the output end of the dynamic loading control part is connected with the dynamic loading generation part and used for outputting the total dynamic loading after coupling to the dynamic loading generation part;
the sintering control system is arranged outside the pressure maintaining cabin, the output end of the sintering control system is connected with the input end of the dynamic loading control part, and the sintering control system is used for regulating and controlling the total applied dynamic loading according to the input sintering process parameters;
and the alternating current control system is arranged outside the pressure maintaining cabin, the input end of the alternating current control system is connected with the output end of the sintering control system, and the output end of the alternating current control system is connected with the dynamic loading generation part and is used for outputting alternating current to the dynamic loading generation part and adjusting the effective value and the frequency of the alternating current according to the input sintering process parameters.
The rapid sintering equipment is characterized in that the dynamic loading generation part preferably comprises an electrode, a pressure head and a die sleeve, the electrode comprises an upper pressure head electrode and a lower pressure head electrode, and the pressure head comprises an upper pressure head and a lower pressure head; the upper end of the upper pressure head electrode penetrates through the bulkhead of the pressure-holding chamber and is fixedly connected with the furnace frame, the lower end of the upper pressure head electrode is connected with the upper end of the upper pressure head, and the lower end of the upper pressure head is a free end; the lower end of the lower pressure head electrode penetrates through the bulkhead of the pressure holding cabin to be connected with the dynamic loading control part, the upper end of the lower pressure head electrode is connected with the lower end of the lower pressure head, and the upper end of the lower pressure head is a free end; the free end of the upper pressure head is positioned right above the free end of the lower pressure head, and a gap is reserved between the free end of the upper pressure head and the free end of the lower pressure head and used for containing sintering materials; the die sleeve is annularly sleeved outside the upper pressure head and the lower pressure head.
The rapid sintering equipment preferably comprises a dynamic loading control part, a loading servo valve and a pressure master control module, wherein the output end of the hydraulic oil cylinder is connected with the lower end of the lower pressure head electrode, and the input end of the hydraulic oil cylinder is connected with the output end of the loading servo valve; the input end of the pressure master control module is connected with the output end of the sintering control system, and the output end of the pressure master control module is connected with the input end of the loading servo valve.
Preferably, the loading servo valve comprises a static loading servo valve and a dynamic loading servo valve, the input ends of the static loading servo valve and the dynamic loading servo valve are respectively connected with the output end of the pressure master control module, and the output ends of the static loading servo valve and the dynamic loading servo valve are respectively connected with the input end of the hydraulic oil cylinder.
Preferably, the output end of the alternating current control system is connected with the upper pressure head electrode and the lower pressure head electrode respectively, and the alternating current control system, the upper pressure head electrode, the lower pressure head electrode, the upper pressure head, the lower pressure head and the mold sleeve form a conductive path.
Preferably, the static loading output by the dynamic loading system of the rapid sintering equipment is 0-100T, T represents ton, the output dynamic loading intensity is 0-5T, and the dynamic loading frequency is 0-100 Hz; and/or the presence of a gas in the gas,
the working voltage of the alternating current control system is 0-100V, and the working current is 0-5000A.
The rapid sintering equipment preferably further comprises an atmosphere control system, which comprises an air inlet and an air outlet and an atmosphere control module, wherein the air inlet and the air outlet are arranged on the bulkhead of the pressure-holding chamber and penetrate through the bulkhead of the pressure-holding chamber, the input end of the atmosphere control module is connected with the output end of the sintering control system, and the output end of the atmosphere control module is connected with the air inlet and the air outlet.
The rapid sintering equipment preferably further comprises a cooling system, wherein the cooling system comprises a cooling water channel and a cooling water control module; the cooling water channel is arranged on the bulkhead of the pressure-holding chamber and is provided with a water inlet and a water outlet, the input end of the cooling water control module is connected with the output end of the sintering control system, and the output end of the cooling water control module is connected with the water inlet.
The rapid sintering equipment preferably further comprises a temperature measuring module which is arranged on the inner bulkhead of the pressure holding chamber and is connected with the sintering control system and used for detecting the surface temperature of the mold sleeve.
The second aspect of the present invention relates to a sintering method for the above-mentioned rapid sintering apparatus dynamically loaded with coupled alternating current, which comprises the following steps:
a, checking the rapid sintering equipment, and putting a material to be sintered;
b, inputting sintering process parameters through the sintering control system;
c, according to the parameter requirements of the sintering process, the sintering control system vacuumizes or injects gas into the pressure-holding chamber through the atmosphere control system, and starts to run a sintering program after the air pressure in the pressure-holding chamber reaches a set value;
d, regulating and controlling parameters for applying total dynamic loading through the sintering control system and the dynamic loading system according to the parameter requirements of the sintering process;
e, adjusting the effective value and frequency of the alternating current through the sintering control system and the alternating current control system according to the parameter requirement of the sintering process, and further adjusting the temperature rise and fall rate and the heat preservation time; detecting the temperature of the surface of the die sleeve through the temperature measuring module;
f, adjusting the sequence of the steps from the step c to the step e according to the parameter requirements of the sintering process, so that the material to be sintered is rapidly sintered under the coupling action of total dynamic loading and alternating current; the cooling water control system is used for adjusting the heat dissipation capacity of the furnace body in the sintering process;
g, after sintering is finished, closing the alternating current control system, and enabling the furnace body to recover normal pressure and unload pressure through the atmosphere control system; and taking out the sintered body after the surface temperature of the die sleeve is reduced to room temperature and the pressure is completely removed, cleaning the interior of the furnace body, closing each working module, and finishing sintering.
In the sintering method, preferably, the sintering process parameters in the step b include dynamic loading parameters, a heating rate, a holding time, a cooling rate and a sintering atmosphere.
In the sintering method, preferably, the parameters of the total dynamic loading in the step d include a mean value, an amplitude, a frequency, a voltage increasing and decreasing rate, and a pressure holding time of the total dynamic loading.
Due to the adoption of the technical scheme, the invention has the following advantages:
1. because the dynamic loading with certain strength and frequency can be coupled on the basis of static loading, compared with the traditional static loading sintering technology, the invention can obviously improve the sintering driving force, reduce the sintering temperature, promote the particle rearrangement in the sintering process, inhibit the grain growth and improve the density of a sintered body, thereby improving the material performance;
2. because the alternating current is adopted to sinter the material to be sintered, compared with the traditional pulse direct current sintering technology, the invention does not need complex rectifying and filtering devices, thereby reducing the total cost of the sintering furnace while having the advantages of ultra-fast heating rate, extremely short sintering time and the like;
3. the invention is favorable for discovering various new scientific phenomena and solving related scientific problems by adopting the advanced sintering technology of dynamic loading and alternating current coupling at home and abroad, promotes the further development of sintering science and technology, and the performance of the prepared sintered body is superior to that of samples prepared by the existing static loading sintering technology and pulse direct current sintering technology, thereby having good industrialized application prospect. In conclusion, the invention can be widely applied to the sintering process of advanced structure and functional materials.
Drawings
FIG. 1 is a schematic structural diagram of a rapid sintering apparatus of the present invention with dynamically loaded coupled alternating current;
FIG. 2 is a schematic diagram illustrating the coupling principle of the total dynamic loading according to the present invention, wherein FIG. 2(a) is a static loading, FIG. 2(b) is a dynamic loading, and FIG. 2(c) is a coupled total dynamic loading;
FIG. 3 is a schematic of an alternating current waveform of the present invention;
the respective symbols in the figure are as follows:
1-furnace body; 2-dynamic loading system, 21-electrode, 211-upper pressure head electrode, 212-lower pressure head electrode, 22-pressure head, 221-upper pressure head, 222-lower pressure head, 23-die sleeve, 24-hydraulic oil cylinder, 25-loading servo valve, 251-static loading servo valve, 252-dynamic loading servo valve and 26-pressure master control module; 3-an alternating current control system; 4-sintering control system; 5-a furnace frame; 6-atmosphere control system, 61-air inlet and outlet, 62-atmosphere control module; 7-cooling system, 71-water inlet, 72-water outlet, 73-cooling water channel, and 74-cooling water control module; and 8-temperature measurement module.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention are described clearly and completely below, and it is obvious that the described embodiments are some, not all embodiments of the present invention. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "inner", "outer", etc. indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the scope of the present invention.
The invention combines the rapid heating alternating current auxiliary sintering technology with the dynamic loading hot pressing sintering technology for the first time, carries out heating sintering by means of Joule heat generated by alternating current passing through materials, can apply dynamic loading with certain frequency and intensity in the sintering process, and breaks through the limitation that the traditional current auxiliary sintering technology can only use static loading.
Example 1
As shown in fig. 1 to 3, the present embodiment provides a rapid sintering apparatus dynamically loaded with a coupled alternating current, comprising the following components:
a furnace frame 5, wherein a furnace body 1 is arranged in the furnace frame 5, and a closed pressure-maintaining cabin is formed in the furnace body 1;
the dynamic loading system 2 comprises a dynamic loading generating part and a dynamic loading control part, wherein the dynamic loading generating part is arranged in the pressure maintaining cabin and is used for pressurizing and heating the sintering material; the output end of the dynamic loading control part is connected with the dynamic loading generating part and is used for outputting the total dynamic loading after coupling to the dynamic loading generating part;
the sintering control system 4 is arranged outside the pressure maintaining cabin, the output end of the sintering control system 4 is connected with the input end of the dynamic loading control part, and the sintering control system 4 is used for regulating and controlling the total dynamic loading applied according to the input sintering process parameters;
and the alternating current control system 3 is arranged outside the pressure maintaining cabin, the input end of the alternating current control system is connected with the output end of the sintering control system 4, and the output end of the alternating current control system is connected with the dynamic loading generation part and is used for outputting alternating current to the dynamic loading generation part and adjusting the effective value and the frequency of the alternating current according to the input sintering process parameters.
In this embodiment, it is preferable that the dynamic loading generating section includes an electrode 21, a ram 22, and a die sleeve 23, the electrode 21 includes an upper ram electrode 211 and a lower ram electrode 212, and the ram 22 includes an upper ram 221 and a lower ram 222; the upper end of the upper pressure head electrode 211 penetrates through the bulkhead of the pressure-holding cabin to be fixedly connected with the furnace frame 5, the lower end of the upper pressure head electrode 211 is connected with the upper end of an upper pressure head 221, and the lower end of the upper pressure head 221 is a free end; the lower end of the lower pressure head electrode 212 passes through the bulkhead of the pressure-holding cabin to be connected with the dynamic loading control part, the upper end of the lower pressure head electrode 212 is connected with the lower end of the lower pressure head 222, and the upper end of the lower pressure head 222 is a free end; the free end of the upper ram 221 is located directly above the free end of the lower ram 222, leaving a gap therebetween for receiving the sintering material; the die sleeve 23 is looped over the exterior of the upper ram 221 and the lower ram 222.
In this embodiment, preferably, the dynamic loading control unit includes a hydraulic oil cylinder 24, a loading servo valve 25 and a pressure master control module 26, an output end of the hydraulic oil cylinder 24 is connected to a lower end of the lower pressure head electrode 212, and an input end thereof is connected to an output end of the loading servo valve 25; the input end of the pressure master control module 26 is connected with the output end of the sintering control system 4, and the output end thereof is connected with the input end of the loading servo valve 25.
In this embodiment, preferably, the loading servo valve 25 includes a static loading servo valve 251 and a dynamic loading servo valve 252, and the input terminals of the static loading servo valve 251 and the dynamic loading servo valve 252 are respectively connected to the output terminal of the pressure master control module 26, and the output terminals of the two are respectively connected to the input terminal of the hydraulic cylinder 24. During operation, the sintering control system 4 sends sintering pressure signals to the pressure master control module 26 according to a preset sintering schedule, wherein the sintering pressure signals comprise a static loading signal with high intensity and a dynamic loading signal with small amplitude and certain frequency; the pressure master control module 26 sends a static loading signal to the static loading servo valve 251 and sends a dynamic loading signal to the dynamic loading servo valve 252 according to the received sintering pressure signal; the static loading servo valve 251 and the dynamic loading servo valve 252 respectively send a static loading signal and a dynamic loading signal to the hydraulic oil cylinder 24 at the same time, the hydraulic oil cylinder 24 couples the received constant pressure signal and the oscillation pressure signal, and the total dynamic loading is output to the lower pressure head electrode 212 after coupling; the coupling principle of the total dynamic loading is shown in fig. 2.
In this embodiment, preferably, the output end of the alternating current control system 3 is connected to the upper ram electrode 211 and the lower ram electrode 212, respectively, and the alternating current control system 3, the upper ram electrode 211, the lower ram electrode 212, the upper ram 221, the lower ram 222, and the mold sleeve 23 form a conductive path. When the sintering control system 4 works, an alternating current signal is sent to the alternating current control system 3 according to a preset sintering schedule, and the alternating current control system 3 regulates alternating current flowing through a conductive path. Joule heat is generated when the alternating current flows through the die sleeve 23 to heat the die sleeve 23, thereby heating the material to be sintered; the waveform of the alternating current is shown in fig. 3.
In this embodiment, preferably, the static loading output by the dynamic loading system 2 is 0 to 100T, T represents "ton", the dynamic loading intensity output is 0 to 5T, and the dynamic loading frequency is 0 to 100 Hz.
In this embodiment, the working voltage of the ac current control system 3 is preferably 0 to 100V, and the working current is preferably 0 to 5000A.
In this embodiment, it is preferable that the atmosphere control system 6 further comprises an air inlet/outlet 61 and an atmosphere control module 62, the air inlet/outlet 61 is disposed on and penetrates through the wall of the ballast, the input end of the atmosphere control module 62 is connected to the output end of the sintering control system 4, and the output end of the atmosphere control module 62 is connected to the air inlet/outlet 61. During operation, the sintering control system 4 sends a vacuum-pumping or gas-filling signal to the atmosphere control module 62, and the atmosphere control module 62 performs vacuum-pumping or gas-filling operation on the furnace body 1 through the gas inlet/outlet hole 61 according to the received signal.
In this embodiment, it is preferable that the cooling system 7 is further included, and the cooling system 7 includes a cooling water passage 73 and a cooling water control module 74; the cooling water channel 73 is arranged on the bulkhead of the holding chamber and is provided with a water inlet 71 and a water outlet 72, the input of the cooling water control module 74 is connected with the output of the sintering control system 4, and the output of the cooling water control module 74 is connected with the water inlet 71. In operation, the cooling water control module 74 adjusts the flow rate of the cooling water in the cooling water channel 73 according to the cooling water circulation signal sent by the sintering control system 4, thereby adjusting and controlling the heat dissipation rate of the furnace body 1.
In this embodiment, it is preferable that the sintering device further comprises a temperature measuring module 8, which is arranged on the inner bulkhead of the pressure holding chamber and connected with the sintering control system 4, for detecting the surface temperature of the mold sleeve 23 and feeding back the temperature measurement value to the sintering control system 4; the sintering control system 4 sends an alternating current signal to the alternating current control system 3 according to the received temperature measurement value feedback, and adjusts the alternating current so as to adjust the temperature of the mold sleeve 23.
In this embodiment, preferably, the temperature measuring module 8 can measure temperature through an infrared temperature measuring device, and can also measure temperature through a high-temperature thermocouple.
In this embodiment, the upper and lower chuck electrodes 211 and 212 are preferably high-strength conductive graphite materials (graphite materials with strength matching with the specific sintering pressure are selected); the upper pressing head 221 and the lower pressing head 222 are made of high-strength conductive graphite materials; the mold sleeve 23 may be selected from a high strength conductive graphite material or other insulating material depending on the conductivity of the material to be sintered.
Example 2
As shown in fig. 1 to 3, the present embodiment relates to a sintering method of a rapid sintering apparatus dynamically loaded with coupled alternating current, comprising the following steps:
a, checking rapid sintering equipment, and putting a material to be sintered;
b, inputting sintering process parameters through a sintering control system 4;
c, according to the parameter requirements of the sintering process, the sintering control system 4 vacuumizes the pressure maintaining cabin or introduces gas (such as argon, nitrogen and the like) through the atmosphere control system 6, and starts to operate a sintering program after the air pressure in the pressure maintaining cabin reaches a set value;
d, regulating and controlling parameters for applying total dynamic loading through a sintering control system 4 and a dynamic loading system 2 according to the parameter requirements of the sintering process;
e, adjusting the effective value and frequency of the alternating current through a sintering control system 4 and an alternating current control system 3 according to the parameter requirements of the sintering process, and further adjusting the temperature rise and fall rate and the heat preservation time; detecting the temperature of the surface of the die sleeve 23 through the temperature measuring module 8;
f, adjusting the sequence of the three steps from the step c to the step e according to the parameter requirements of the sintering process, so that the material to be sintered is rapidly sintered under the coupling action of total dynamic loading and alternating current; the heat dissipation capacity of the furnace body 1 is adjusted through the cooling water control system 7 in the sintering process;
g, after sintering is finished, closing the alternating current control system 3, and recovering the normal pressure in the furnace body 1 through the atmosphere control system 6 to unload the pressure; and taking out the sintered body after the surface temperature of the die sleeve 23 is reduced to room temperature and the pressure is completely removed, cleaning the interior of the furnace body 1, closing each working module, and finishing sintering.
In this embodiment, preferably, the sintering process parameters in step b include dynamic loading parameters, a temperature rise rate, a temperature holding time, a temperature decrease rate, and a sintering atmosphere.
In this embodiment, preferably, the parameters of the total dynamic loading in step d include a mean value, an amplitude, a frequency, a buck-boost speed and a dwell time of the total dynamic loading.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (11)

1. A rapid sintering device for dynamically loading coupled alternating current is characterized by comprising the following components:
the furnace comprises a furnace frame (5), wherein a furnace body (1) is arranged in the furnace frame (5), and a closed pressure-maintaining cabin is formed in the furnace body (1);
the dynamic loading system (2) comprises a dynamic loading generation part and a dynamic loading control part, wherein the dynamic loading generation part is arranged in the pressure maintaining cabin and is used for pressurizing and heating the sintering material; the dynamic loading control part is arranged outside the pressure maintaining cabin, and the output end of the dynamic loading control part is connected with the dynamic loading generation part and used for outputting the total dynamic loading after coupling to the dynamic loading generation part;
the sintering control system (4) is arranged outside the pressure maintaining cabin, the output end of the sintering control system (4) is connected with the input end of the dynamic loading control part, and the sintering control system (4) is used for regulating and controlling the total applied dynamic loading according to the input sintering process parameters;
and the alternating current control system (3) is arranged outside the pressure maintaining cabin, the input end of the alternating current control system is connected with the output end of the sintering control system (4), and the output end of the alternating current control system is connected with the dynamic loading generation part and is used for outputting alternating current to the dynamic loading generation part and adjusting the effective value and the frequency of the alternating current according to the input sintering process parameters.
2. The rapid sintering apparatus according to claim 1, wherein the dynamic loading generating section comprises an electrode (21), a ram (22) and a die sleeve (23), the electrode (21) comprises an upper ram electrode (211) and a lower ram electrode (212), the ram (22) comprises an upper ram (221) and a lower ram (222); the upper end of the upper pressure head electrode (211) penetrates through the bulkhead of the pressure holding chamber to be fixedly connected with the furnace frame (5), the lower end of the upper pressure head electrode (211) is connected with the upper end of the upper pressure head (221), and the lower end of the upper pressure head (221) is a free end; the lower end of the lower pressure head electrode (212) penetrates through the bulkhead of the pressure holding chamber to be connected with the dynamic loading control part, the upper end of the lower pressure head electrode (212) is connected with the lower end of the lower pressure head (222), and the upper end of the lower pressure head (222) is a free end; the free end of the upper pressure head (221) is positioned right above the free end of the lower pressure head (222), and a gap is reserved between the free end of the upper pressure head and the free end of the lower pressure head for containing sintering materials; the die sleeve (23) is sleeved outside the upper press head (221) and the lower press head (222).
3. The rapid sintering equipment according to claim 1, wherein the dynamic loading control part comprises a hydraulic oil cylinder (24), a loading servo valve (25) and a pressure master control module (26), the output end of the hydraulic oil cylinder (24) is connected with the lower end of the lower pressure head electrode (212), and the input end of the hydraulic oil cylinder is connected with the output end of the loading servo valve (25); the input end of the pressure master control module (26) is connected with the output end of the sintering control system (4), and the output end of the pressure master control module is connected with the input end of the loading servo valve (25).
4. The rapid sintering equipment according to claim 3, characterized in that the loading servo valve (25) comprises a static loading servo valve (251) and a dynamic loading servo valve (252), wherein the input ends of the static loading servo valve (251) and the dynamic loading servo valve (252) are respectively connected with the output end of the pressure master control module (26), and the output ends of the static loading servo valve (251) and the dynamic loading servo valve are respectively connected with the input end of the hydraulic oil cylinder (24).
5. The rapid sintering apparatus according to claim 2, wherein the output end of the alternating current control system (3) is connected with the upper ram electrode (211) and the lower ram electrode (212), respectively, and the alternating current control system (3), the upper ram electrode (211), the lower ram electrode (212), the upper ram (221), the lower ram (222) and the mold sleeve (23) constitute a conductive path.
6. The rapid sintering equipment according to claim 1, wherein the static loading output by the dynamic loading system (2) is 0-100T, T is "ton", the dynamic loading intensity output is 0-5T, and the dynamic loading frequency is 0-100 Hz; and/or the presence of a gas in the gas,
the working voltage of the alternating current control system (3) is 0-100V, and the working current is 0-5000A.
7. The rapid sintering apparatus according to claim 1, further comprising an atmosphere control system (6) comprising an air inlet and outlet (61) and an atmosphere control module (62), wherein the air inlet and outlet (61) is disposed on and extends through a wall of the ballast, an input of the atmosphere control module (62) is connected to an output of the sintering control system (4), and an output of the atmosphere control module (62) is connected to the air inlet and outlet (61).
8. The rapid sintering apparatus according to claim 1, further comprising a cooling system (7), the cooling system (7) comprising a cooling water channel (73) and a cooling water control module (74); the cooling water channel (73) is arranged on the bulkhead of the pressure-holding chamber and is provided with a water inlet (71) and a water outlet (72), the input end of the cooling water control module (74) is connected with the output end of the sintering control system (4), and the output end of the cooling water control module (74) is connected with the water inlet (71).
9. The rapid sintering apparatus according to claim 1, further comprising a temperature measurement module (8) disposed on an inner bulkhead of the pressure holding chamber and connected to the sintering control system (4) for detecting a surface temperature of the mold sleeve (23).
10. A sintering method of a rapid sintering apparatus dynamically loaded with coupled alternating current according to any one of claims 2 to 9, comprising the steps of:
a, checking the rapid sintering equipment, and putting a material to be sintered;
b, inputting sintering process parameters through the sintering control system (4);
c, according to the parameter requirements of the sintering process, the sintering control system (4) vacuumizes or injects gas into the pressure-maintaining cabin through the atmosphere control system (6), and starts to operate a sintering program after the air pressure in the pressure-maintaining cabin reaches a set value;
d, regulating and controlling parameters for applying total dynamic loading through the sintering control system (4) and the dynamic loading system (2) according to the parameter requirements of the sintering process;
e, adjusting the effective value and frequency of the alternating current through the sintering control system (4) and the alternating current control system (3) according to the parameter requirements of the sintering process, and further adjusting the temperature rising and reducing rate and the heat preservation time; detecting the temperature of the surface of the die sleeve (23) through the temperature measuring module (8);
f, adjusting the sequence of the steps from the step c to the step e according to the parameter requirements of the sintering process, so that the material to be sintered is rapidly sintered under the coupling action of total dynamic loading and alternating current; the heat dissipation capacity of the furnace body (1) is adjusted through the cooling water control system (7) in the sintering process;
g, after sintering is finished, closing the alternating current control system (3), and recovering normal pressure and unloading pressure in the furnace body (1) through the atmosphere control system (6); and taking out the sintered body after the surface temperature of the die sleeve (23) is reduced to room temperature and the pressure is completely removed, cleaning the interior of the furnace body (1), closing each working module, and finishing sintering.
11. The sintering method according to claim 10, wherein the sintering process parameters in the step b comprise dynamic loading parameters, heating rate, holding time, cooling rate and sintering atmosphere;
the parameters of the total dynamic loading in the step d comprise the mean value, the amplitude, the frequency, the voltage increasing and decreasing rate and the pressure maintaining time of the total dynamic loading.
CN202010749837.1A 2020-07-30 2020-07-30 Rapid sintering equipment and sintering method for dynamically loading coupled alternating current Pending CN111912227A (en)

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Application publication date: 20201110