CN105135873A - Dynamic pressure electric pulse double-field control sintering furnace and sintering method - Google Patents

Dynamic pressure electric pulse double-field control sintering furnace and sintering method Download PDF

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CN105135873A
CN105135873A CN201510473828.3A CN201510473828A CN105135873A CN 105135873 A CN105135873 A CN 105135873A CN 201510473828 A CN201510473828 A CN 201510473828A CN 105135873 A CN105135873 A CN 105135873A
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dynamic pressure
sintering
control
vacuum
sintered
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CN105135873B (en
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谢志鹏
韩耀
李双
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Tsinghua University
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Tsinghua University
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Abstract

The invention relates to a dynamic pressure electric pulse double-field control sintering furnace and a sintering method. The sintering furnace comprises a furnace body, a dynamic pressure system, a pulse current generator and a sintering controller. The furnace body is connected with the dynamic pressure system and the pulse current generator. The dynamic pressure system and the pulse current generator are both connected to the sintering controller. A die is arranged in the furnace body. The dynamic pressure system comprises an upper press head electrode, a lower press head electrode, an upper press head, a lower press head, a constant pressure control module, a dynamic pressure control module and a pressure master control module. The dynamic pressure system is connected with the sintering controller. The pulse current generator is connected with the upper press head electrode and the lower press head electrode and connected with the sintering controller as well. The sintering controller controls the dynamic pressure system and the pulse current generator to generate the adjustable dynamic pressure for a material to be sintered and conduct plasma pulse current sintering on the material to be sintered. The dynamic pressure electric pulse double-field control sintering furnace and the sintering method can be widely applied to sintering of the high-performance material.

Description

A kind of dynamic pressure electric pulse two fields control sintering furnace and sintering method
Technical field
The present invention relates to a kind of sintering furnace and sintering method, particularly about a kind of dynamic pressure electric pulse two fields control sintering furnace and sintering method.
Background technology
Sintering process in advanced material preparation process realizes the committed step that particle is densified, give mechanical strength.The fusing point of pottery and some metal material is higher, is often difficult to realize sintering densification, therefore proposes higher requirement to agglomerating plant and technology.
At present conventional sintering method comprises normal pressure-sintered, hot pressed sintering two kinds and discharge plasma sintering.Normal pressure-sintered is simple high temperature sintering methods, and promote densifying materials by heating at atmosheric pressure, the densification degree of material is not high.Hot pressed sintering is sintering while, unidirectional or two-way pressure is applied to powder, accelerate densification process, compare normal pressure-sintered, the temperature of hot pressed sintering is lower, sintering time is shorter, and effectively can promote densified, the inhibiting grain growth of material, current application comprises advanced ceramics, carbide alloy, powder metallurgy and composite etc.Discharge plasma sintering is a kind of new material sintering preparation method that development in recent years is got up, also known as pulse electric current sintering.The main feature of this technology passes into DC pulse current to electrode, instantaneous generation discharge plasma, effectively utilize the surface activation that pulse current and particle self-heating produce, realize the supper-fast densification sintering of material, substantially reduce sintering time, reduce sintering temperature, but pulse current has strong directionality and polarity, cause the material after sintering to there will be performance profile along current electric fields direction uneven, affect the use of material.Research shows that the pressure that current agglomerating plant provides is constant pressure, under constant pressure effect particle be difficult to slippage rearrangement, pore be difficult to discharge, easily " hard aggregation " is produced between particle in sintering process, easily cause the non-uniform phenomenon of microstructure, therefore the raising of the densified degree of sintered body and mechanical property is constrained, and in sintering process, the situation of powder contraction, densifying materials cannot be grasped in time, thus constrains the sintering of high performance material.
Summary of the invention
For the problems referred to above, the object of this invention is to provide and a kind ofly effectively can improve the electric field and temperature field non-uniform phenomenon that occur in discharge plasma sintering, electric field and dynamic force field is made to be in controlled change, reduce and eliminate " hard aggregation ", realize material quick densifying at a lower temperature, improve powder bulk density, promote that pore is discharged, thus dynamic pressure electric pulse two fields control sintering furnace of the high-quality performance materials such as preparation high density, low defect, high strength and sintering method.
For achieving the above object, the present invention takes following technical scheme: a kind of dynamic pressure electric pulse two field control sintering furnace, is characterized in that: it comprises body of heater, dynamic pressure system, impulse current generator and sintering controller; Described body of heater connects described dynamic pressure system and described impulse current generator, and described dynamic pressure system and described impulse current generator are all connected described sintering controller;
Described furnace interior is provided with mould, and described mould adopts the column structure with hollow cavity;
Described dynamic pressure system comprises seaming chuck electrode, push-down head electrode, seaming chuck, push-down head, constant pressure control module, dynamic pressure control module and pressure top control module; Described seaming chuck electrode, described push-down head electrode are separately fixed at described upper of furnace body and described lower portion of furnace body; Described seaming chuck one end connects described seaming chuck electrode base, and the other end inserts described mould hollow cavity top; Described push-down head one end connects described push-down head electrode, and the other end inserts bottom described mould hollow cavity, and has the space holding material to be sintered between described seaming chuck end in described mould hollow cavity and described push-down head end; Described seaming chuck top of electrodes is connected with described constant pressure control module and described dynamic pressure control module, and described constant pressure control module and described dynamic pressure control module are all connected to described pressure top control module; Described pressure top control module connects the output of described sintering controller, dynamic pressure control signal is sent to described pressure top control module by described sintering controller, described pressure top control module controls according to the dynamic pressure control signal received constant pressure that described constant pressure control module produces and the dynamic pressure that the dynamic pressure that described dynamic pressure control module produces is superposed to a frequency and adjustable amplitude acts on described seaming chuck electrode, and then controls described seaming chuck by described seaming chuck electrode and treat agglomerated material and produce the adjustable dynamic pressure of size.
The output of described impulse current generator connects described seaming chuck electrode and described push-down head electrode, the input of described impulse current generator is connected to the output of described sintering controller, pulse current control signal is sent to described impulse current generator by described sintering controller, described impulse current generator carries out plasma pulse electric current sintering according to the pulse current control signal received to described seaming chuck electrode and described push-down head electrode, plasma pulse electric current is by described seaming chuck electrode, described push-down head electrode, described seaming chuck and described push-down head act on material to be sintered.
Described dynamic pressure electric pulse two field control sintering furnace also comprises cooling water system, described cooling water system comprises water-cooling channel and cooling water control system, described water-cooling channel is positioned at described furnace interior and close described body of heater wall, the delivery port of described water-cooling channel is arranged on described body of heater upper end, the water inlet of described water-cooling channel is arranged on described body of heater lower end, the water inlet of described water-cooling channel connects described sintering controller through described cooling water control system, cooling water control signal is sent to described cooling water control system by described sintering controller, described cooling water control system controls inflow and the outflow of cooling water in described water-cooling channel according to the cooling water control signal received.
Described dynamic pressure electric pulse two field control sintering furnace also comprises magnetic grid linear movement measuring system, described magnetic grid linear movement measuring system comprises magnetic head, magnetic grid linear movement pick-up and displacement display, described magnetic head gathers axial displacement signal on the pressure spot of described seaming chuck electrode, the axial displacement signal of acquisition is transferred to described magnetic grid linear movement pick-up, and the axial displacement data collected are delivered to institute's displacement display and show in real time by described magnetic grid linear movement pick-up.
Described dynamic pressure electric pulse two field control sintering furnace also comprises vacuum-control(led) system, described body of heater connects described sintering controller through described vacuum-control(led) system, vacuum control signal is sent to described vacuum-control(led) system by described sintering controller, and described vacuum-control(led) system regulates the vacuum in described body of heater according to the vacuum control signal received; Described vacuum-control(led) system comprises mechanical pump, lobe pump, pressure vacuum gauge and magnetic valve.
Described mould adopts carbon/carbon compound material.
The dynamic pressure magnitude range that described dynamic pressure control module produces is 0 ~ 5MPa, and adjustable frequency scope is 0 ~ 3Hz.
Use a sintering method for dynamic pressure electric pulse two field control sintering furnace, comprise the following steps:
1) detect power supply, water source and vacuum, material to be sintered is positioned in the hollow bulb inner chamber of body of heater inner mold;
2) vacuum in material technology to be sintered requirement is reached by the vacuum-control(led) system vacuum controlled in body of heater;
3) controlled the dynamic pressure of dynamic pressure systemic effect frequency and amplitude needed for the material to be sintered by sintering controller, dynamic pressure promotes the particle re-arrangement of material to be sintered, thus improves the green density of material to be sintered;
4) while treating agglomerated material effect dynamic pressure, treat agglomerated material by sintering controller control impuls current feedback circuit and carry out plasma pulse electric current sintering, make material to be sintered be subject to two fields control comprehensive function of dynamic pressure and plasma pulse electric current simultaneously;
5) and the technological requirement time temperature required according to material to be sintered, when material to be sintered reach temperature required after, keep material technology to be sintered to want seeking time;
6), after material technology to be sintered wants seeking time to reach, controlled the inlet and outlet of cooling water in water-cooling channel by cooling water system, and then slow cooling is carried out to body of heater; Simultaneously by sintering controller controlled pressure top control module, slowly reduce dynamic pressure until dynamic pressure is zero;
7) after the temperature cooling in body of heater reaches room temperature, sintering completes, and is taken out by sintered body in body of heater.
The present invention is owing to taking above technical scheme, it has the following advantages: 1, the present invention carries out plasma pulse electric current sintering owing to adopting impulse current generator to treat agglomerated material, and treat agglomerated material by dynamic pressure system and apply a dynamic pressure, two fields control comprehensive function of dynamic pressure and plasma pulse electric current can reduce sintering temperature needed for material to be sintered and sintering time greatly, promote the particle re-arrangement of material to be sintered, particle migration and pore are discharged, accelerate the volume contraction of material to be sintered, reduce and eliminate " hard aggregation ", can quick densifying, eliminate pore, the defects such as micro-crack, greatly improve sintered density and the performance of goods.2, the present invention produces dynamic pressure owing to adopting constant pressure and dynamic pressure superposition, and the dynamic pressure frequency that material to be sintered is obtained and the equal controllable of size, meet the technological requirement of material to be sintered.In sum, the present invention can be widely used in preparing in the sintering process of high performance material.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of dynamic pressure electric pulse of the present invention two field control sintering furnace
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described in detail.
As shown in Figure 1, the invention provides a kind of dynamic pressure electric pulse two field control sintering furnace, it comprises body of heater 1, dynamic pressure system 2, impulse current generator 3 and sintering controller 4.Body of heater 1 connects dynamic pressure system 2 and impulse current generator 3, and dynamic pressure system 2 and impulse current generator 3 are all connected sintering controller 4.
Body of heater 1 inside is provided with mould 11, and mould 11 adopts the column structure with hollow cavity, and material to be sintered is positioned in the hollow cavity of mould 11.
Dynamic pressure system 2 comprises seaming chuck electrode 21, push-down head electrode 22, seaming chuck 23, push-down head 24, constant pressure control module 25, dynamic pressure control module 26 and pressure top control module 27.Seaming chuck electrode 21, push-down head electrode 22 are separately fixed at body of heater 1 upper and lower, and seaming chuck 23 one end connects bottom seaming chuck electrode 21, and the other end inserts mould 11 hollow cavity top; Push-down head 24 one end connects push-down head electrode 22, and the other end inserts bottom hollow cavity, and has the space holding material to be sintered between seaming chuck 23 end in mould 11 hollow cavity and push-down head 24 end.Seaming chuck electrode 21 top is connected with constant pressure control module 25 and dynamic pressure control module 26, and constant pressure control module 25 and dynamic pressure control module 26 are all connected to pressure top control module 27.Pressure top control module 27 connects the output of sintering controller 4, dynamic pressure control signal is sent to pressure top control module 27 by sintering controller 4, pressure top control module 27 controls according to the dynamic pressure control signal that receives the dynamic pressure that constant pressure that constant pressure control module 25 produces and the dynamic pressure that dynamic pressure control module 26 produces be superposed to a frequency and adjustable amplitude and acts on seaming chuck electrode 21, and then controls seaming chuck 23 by seaming chuck electrode 21 and treat agglomerated material and produce the adjustable dynamic pressure of size.
The output of impulse current generator 3 connects seaming chuck electrode 21 and push-down head electrode 22, the input of impulse current generator 3 is connected to the output of sintering controller 4, pulse current control signal is sent to impulse current generator 3 by sintering controller 4, impulse current generator 3 carries out plasma pulse electric current sintering according to the pulse current control signal received to seaming chuck electrode 21 and push-down head electrode 22, plasma pulse electric current is by seaming chuck electrode 21, seaming chuck 23, push-down head electrode 22 and push-down head 24, instantaneous generation discharge plasma when arriving material to be sintered, material to be sintered self is made to produce Joule heat and the surface particles of material to be sintered is activated, the energy produced transmits between the particle of material to be sintered, accelerate the diffusion of energy at storeroom to be sintered, make material to be sintered be subject to two fields control comprehensive function of dynamic pressure and plasma pulse electric current simultaneously.
In above-described embodiment, dynamic pressure electric pulse two field control sintering furnace also comprises cooling water system, cooling water system comprises water-cooling channel 51 and cooling water control system 52, water-cooling channel 51 is positioned at body of heater 1 inside and close body of heater 1 wall, the delivery port 53 of water-cooling channel 51 is arranged on body of heater 1 upper end, the water inlet 54 of water-cooling channel 51 is arranged on body of heater 1 lower end, the water inlet 54 of water-cooling channel 51 connects sintering controller 4 through cooling water control system 52, cooling water control signal is sent to cooling water control system 52 by sintering controller 4, cooling water control system 52 controls inflow and the outflow of cooling water in water-cooling channel 51 according to the cooling water control signal received.
In above-described embodiment, dynamic pressure electric pulse two field control sintering furnace also comprises magnetic grid linear movement measuring system 6, magnetic grid linear movement measuring system 6 comprises magnetic head 61, magnetic grid linear movement pick-up 62 and displacement display 63, magnetic head 61 directly gathers axial displacement signal on the pressure spot of seaming chuck electrode 23, the axial displacement signal of acquisition is transferred to magnetic grid linear movement pick-up 62, and the axial displacement data collected are delivered to displacement display 63 and show in real time by magnetic grid linear movement pick-up 62.
In above-described embodiment, dynamic pressure electric pulse two field control sintering furnace also comprises vacuum-control(led) system 7, body of heater 1 connects sintering controller 4 through vacuum-control(led) system 7, vacuum control signal is sent to vacuum-control(led) system 7 by sintering controller 4, vacuum-control(led) system 7 regulates the vacuum in body of heater 1 according to the vacuum control signal received, and vacuum-control(led) system 7 comprises mechanical pump, lobe pump, pressure vacuum gauge and magnetic valve.
In above-described embodiment, mould 11 adopts toughness and the higher carbon/carbon compound material of intensity, and can bear high frequency dynamic pressure constant impingement, life cycle is long.
In above-described embodiment, the dynamic pressure magnitude range that dynamic pressure control module 26 produces is 0 ~ 5MPa, and adjustable frequency scope is 0 ~ 3Hz.
The present invention also provides a kind of dynamic pressure electric pulse two field control sintering method, comprises the following steps:
1) detect power supply, water source and vacuum, material to be sintered is positioned in the hollow bulb inner chamber of mould 11.
2) vacuum in material technology to be sintered requirement is reached by vacuum-control(led) system 7 vacuum controlled in body of heater 1.
3) control by sintering controller 4 dynamic pressure that dynamic pressure system 2 acts on frequency and amplitude needed for material to be sintered, dynamic pressure promotes the particle re-arrangement of material to be sintered, thus improves the green density of material to be sintered.
4) while treating agglomerated material effect dynamic pressure, treat agglomerated material by sintering controller 4 control impuls current feedback circuit 3 and carry out plasma pulse electric current sintering, make material to be sintered be subject to two fields control comprehensive function of dynamic pressure and plasma pulse electric current simultaneously.
5) and the technological requirement time temperature required according to material to be sintered, when material to be sintered reach temperature required after, keep material technology to be sintered to want seeking time.
6), after material technology to be sintered wants seeking time to reach, controlled the inlet and outlet of cooling water in water-cooling channel 11 by cooling water system, and then slow cooling is carried out to body of heater 1; Simultaneously by sintering controller 4 controlled pressure top control module 27, slowly reduce dynamic pressure until dynamic pressure is zero.
7) after the temperature cooling in body of heater 1 reaches room temperature, sintering completes, and is taken out by sintered body in body of heater 1.
The various embodiments described above are only for illustration of the present invention; wherein the structure of each parts, connected mode and manufacture craft etc. all can change to some extent; every equivalents of carrying out on the basis of technical solution of the present invention and improvement, all should not get rid of outside protection scope of the present invention.

Claims (10)

1. dynamic pressure electric pulse two field control sintering furnace, is characterized in that: it comprises body of heater, dynamic pressure system, impulse current generator and sintering controller; Described body of heater connects described dynamic pressure system and described impulse current generator, and described dynamic pressure system and described impulse current generator are all connected described sintering controller;
Described furnace interior is provided with mould, and described mould adopts the column structure with hollow cavity;
Described dynamic pressure system comprises seaming chuck electrode, push-down head electrode, seaming chuck, push-down head, constant pressure control module, dynamic pressure control module and pressure top control module; Described seaming chuck electrode, described push-down head electrode are separately fixed at described upper of furnace body and described lower portion of furnace body; Described seaming chuck one end connects described seaming chuck electrode base, and the other end inserts described mould hollow cavity top; Described push-down head one end connects described push-down head electrode, and the other end inserts bottom described mould hollow cavity, and has the space holding material to be sintered between described seaming chuck end in described mould hollow cavity and described push-down head end; Described seaming chuck top of electrodes is connected with described constant pressure control module and described dynamic pressure control module, and described constant pressure control module and described dynamic pressure control module are all connected to described pressure top control module; Described pressure top control module connects the output of described sintering controller, dynamic pressure control signal is sent to described pressure top control module by described sintering controller, described pressure top control module controls according to the dynamic pressure control signal received constant pressure that described constant pressure control module produces and the dynamic pressure that the dynamic pressure that described dynamic pressure control module produces is superposed to a frequency and adjustable amplitude acts on described seaming chuck electrode, and then controls described seaming chuck by described seaming chuck electrode and treat agglomerated material and produce the adjustable dynamic pressure of size.
2. a kind of dynamic pressure electric pulse as claimed in claim 1 two field control sintering furnace, it is characterized in that: the output of described impulse current generator connects described seaming chuck electrode and described push-down head electrode, the input of described impulse current generator is connected to the output of described sintering controller, pulse current control signal is sent to described impulse current generator by described sintering controller, described impulse current generator carries out plasma pulse electric current sintering according to the pulse current control signal received to described seaming chuck electrode and described push-down head electrode, plasma pulse electric current is by described seaming chuck electrode, described push-down head electrode, described seaming chuck and described push-down head act on material to be sintered.
3. a kind of dynamic pressure electric pulse as claimed in claim 1 or 2 two field control sintering furnace, it is characterized in that: described dynamic pressure electric pulse two field control sintering furnace also comprises cooling water system, described cooling water system comprises water-cooling channel and cooling water control system, described water-cooling channel is positioned at described furnace interior and close described body of heater wall, the delivery port of described water-cooling channel is arranged on described body of heater upper end, the water inlet of described water-cooling channel is arranged on described body of heater lower end, the water inlet of described water-cooling channel connects described sintering controller through described cooling water control system, cooling water control signal is sent to described cooling water control system by described sintering controller, described cooling water control system controls inflow and the outflow of cooling water in described water-cooling channel according to the cooling water control signal received.
4. a kind of dynamic pressure electric pulse as claimed in claim 1 or 2 two field control sintering furnace, it is characterized in that: described dynamic pressure electric pulse two field control sintering furnace also comprises magnetic grid linear movement measuring system, described magnetic grid linear movement measuring system comprises magnetic head, magnetic grid linear movement pick-up and displacement display, described magnetic head gathers axial displacement signal on the pressure spot of described seaming chuck electrode, the axial displacement signal of acquisition is transferred to described magnetic grid linear movement pick-up, the axial displacement data collected are delivered to institute's displacement display and show in real time by described magnetic grid linear movement pick-up.
5. a kind of dynamic pressure electric pulse as claimed in claim 3 two field control sintering furnace, it is characterized in that: described dynamic pressure electric pulse two field control sintering furnace also comprises magnetic grid linear movement measuring system, described magnetic grid linear movement measuring system comprises magnetic head, magnetic grid linear movement pick-up and displacement display, described magnetic head gathers axial displacement signal on the pressure spot of described seaming chuck electrode, the axial displacement signal of acquisition is transferred to described magnetic grid linear movement pick-up, the axial displacement data collected are delivered to institute's displacement display and show in real time by described magnetic grid linear movement pick-up.
6. the two field control of a kind of dynamic pressure electric pulse as described in claim 1 or 2 or 5 sintering furnace, it is characterized in that: described dynamic pressure electric pulse two field control sintering furnace also comprises vacuum-control(led) system, described body of heater connects described sintering controller through described vacuum-control(led) system, vacuum control signal is sent to described vacuum-control(led) system by described sintering controller, and described vacuum-control(led) system regulates the vacuum in described body of heater according to the vacuum control signal received; Described vacuum-control(led) system comprises mechanical pump, lobe pump, pressure vacuum gauge and magnetic valve.
7. a kind of dynamic pressure electric pulse as claimed in claim 3 two field control sintering furnace, it is characterized in that: described dynamic pressure electric pulse two field control sintering furnace also comprises vacuum-control(led) system, described body of heater connects described sintering controller through described vacuum-control(led) system, vacuum control signal is sent to described vacuum-control(led) system by described sintering controller, and described vacuum-control(led) system regulates the vacuum in described body of heater according to the vacuum control signal received; Described vacuum-control(led) system comprises mechanical pump, lobe pump, pressure vacuum gauge and magnetic valve.
8. the two field control of a kind of dynamic pressure electric pulse as described in claim 1 or 2 or 5 or 7 sintering furnace, is characterized in that: described mould adopts carbon/carbon compound material.
9. the two field control of a kind of dynamic pressure electric pulse as described in claim 1 or 2 or 5 or 7 sintering furnace, is characterized in that: the dynamic pressure magnitude range that described dynamic pressure control module produces is 0 ~ 5MPa, and adjustable frequency scope is 0 ~ 3Hz.
10. use a sintering method for the two field control of the dynamic pressure electric pulse according to any one of claim 1 ~ 9 sintering furnace, comprise the following steps:
1) detect power supply, water source and vacuum, material to be sintered is positioned in the hollow bulb inner chamber of body of heater inner mold;
2) vacuum in material technology to be sintered requirement is reached by the vacuum-control(led) system vacuum controlled in body of heater;
3) controlled the dynamic pressure of dynamic pressure systemic effect frequency and amplitude needed for the material to be sintered by sintering controller, dynamic pressure promotes the particle re-arrangement of material to be sintered, thus improves the green density of material to be sintered;
4) while treating agglomerated material effect dynamic pressure, treat agglomerated material by sintering controller control impuls current feedback circuit and carry out plasma pulse electric current sintering, make material to be sintered be subject to two fields control comprehensive function of dynamic pressure and plasma pulse electric current simultaneously;
5) and the technological requirement time temperature required according to material to be sintered, when material to be sintered reach temperature required after, keep material technology to be sintered to want seeking time;
6), after material technology to be sintered wants seeking time to reach, controlled the inlet and outlet of cooling water in water-cooling channel by cooling water system, and then slow cooling is carried out to body of heater; Simultaneously by sintering controller controlled pressure top control module, slowly reduce dynamic pressure until dynamic pressure is zero;
7) after the temperature cooling in body of heater reaches room temperature, sintering completes, and is taken out by sintered body in body of heater.
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