CN103819202B - A kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method - Google Patents
A kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method Download PDFInfo
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- CN103819202B CN103819202B CN201410014329.3A CN201410014329A CN103819202B CN 103819202 B CN103819202 B CN 103819202B CN 201410014329 A CN201410014329 A CN 201410014329A CN 103819202 B CN103819202 B CN 103819202B
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Abstract
The invention discloses a kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method, be called for short the field control sintering such as two; It is characterized in that, comprise ceramic body preparation, the field such as two control sintering oven, ceramic sintered bodies processing, the field control sintering method such as two; Describedly two wait field to control sintering oven to comprise lower furnace body, thermopair, upper furnace body, battery lead plate, bench insulator, contact conductor, graphite packing, control electric field, rubber sealing boot, insulation ring seat, tensimeter, gas cylinder, air valve, compressor, gas inlet and outlet, impulse current generator, sintering controller and fixed feet; The field control sintering method such as two, by applying the comprehensive action of plasma discharging pulsed current, alternating electromagnetic field and gas isostatic pressed to base substrate, makes both macro and micro stupalith be tending towards uniformity in heat energy, pressure and electromagnetic field transmission and direction; Even, isotropic sintering is there is at stupalith microcosmic lattice, crystal boundary and dot matrix, thus the raising of implementation structure stupalith sintering properties.
Description
Technical field
The present invention relates to a kind of superhard wear stupalith manufacturing technology field, be specifically related to a kind of sintering process and technical equipment of stupalith, particularly a kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method.
Background technology
Along with the develop rapidly of electronic industry and space industry in recent years, the manufacturer of ceramic part also gets more and more.Particularly the development of superhard wear stupalith is faster, but the supplementary material formula of superhard wear stupalith, manufacture craft, shaping and sintering method, plays a part very crucial to the quality of superhard wear stupalith and performance.Different according to product structure, specification, precision and performance, prior art commonly uses forming method to be had: the forming methods such as compression moulding, roll forming, extrusion molding, injection forming, hot-injection molding, injection molding and static pressure method.The new forming technique that development in recent years is got up: in-situ consolidation forming technology, rapid shaping technique and nano material forming technique; The sintering method that prior art is commonly used has: pressureless sintering, liquid phase sintering, reaction sintering, explosive sintering method, HIP sintering, microwave sintering method, laser sintered method, discharge plasma sintering method.
The sintering of pottery must possess two primary conditions: (1) exists the chance of material transport; (2) there is a kind of energy, as heat energy, promote and maintain the migration of material.The technology such as existing solid state sintering, liquid phase sintering, reaction sintering, the material structure utilized and the motivating force of sintering different, have their own characteristics each; Main sintering mechanism is liquid phase sintering and solid state sintering; The sintering of traditional ceramics and the electronic ceramics sintering of the overwhelming majority depend on liquid phase sintering, viscous flow and dissolve deposition process again; The sintering of high-strength structure pottery, then based on solid state sintering, carries out material transport by grain boundary decision or dot matrix diffusion, realizes sintering.
In prior art, forming method and sintering method, in the migration of material, use External Force Acting or interior microscopic diffusion; Selected energy mode is heat energy, luminous energy, polarization energy, electric energy; The external pressure provided take isostatic pressing technology as optimal selection; The energy mode provided then with plasma discharge technology for optimal selection; And the crystal boundary of inside is substantially identical with the diffusion of dot matrix; The effect of its energy and external force is all subject to conducting, the restriction of directivity, functioning efficiency and can not give play to effect completely, the defect place of existing shaping and sintering technology development that Here it is.Traditional method often causes the problems such as material internal lack of homogeneity, formed precision are low, and amount of machining is large, and cause stupalith defect many, reliability is low, manufacturing cost is high, seriously hinders high-performance ceramic industrialization and application.
Sintering is a kind of technology utilizing heat energy to make powder green bodies densification.Its definition refers to vesicular ceramic body under the high temperature conditions, the densification process that surface-area reduces, porosity reduces, mechanical property improves; The Macrocosm and microcosm mechanism of action of base substrate in high temperature sintering process and Changing Pattern improve the quality of products, and reduces fuel consumption, obtain the prerequisite of good economic benefit; Total be exactly the minimizing of sintering motivating force interfacial energy, the reduction of the densification of stupalith, grain growth, interfacial energy.
Pressureless sintering: simple high temperature sintering methods, shortcoming is the effect not having external force, and in simple base substrate, heat energy is on Macrocosm and microcosm impact in stupalith; Shortcoming is: pull-out gas and lattice, that crystal boundary resets densification is inadequate.
Hot pressed sintering: simultaneously hot pressed sintering applies pressure to blank in sintering process, accelerates the process of densification.So the temperature of hot pressed sintering is lower, sintering time is shorter.Hot-pressing technique has many decades history, the earliest for the preparation of wolfram varbide and tungsten powder compact piece, has been widely used in now the production of pottery, powder metallurgy and matrix material; Shortcoming is: mechanical system applies pressure, and institute's applied pressure has directivity, and the pressure direction of macroscopic view causes the structural pressure of microcosmic uneven, makes sintered compact performance uniformity bad.
HIP sintering is by powder compact or loads in the powder loading high pressure vessel of jacket, makes powder stand the effect of high temperature and equalized pressure, is sintered into compact piece.Using gas or liquid as pressure medium, make material (powder, base substrate or sintered compact) in heat-processed, stand each pressure to equilibrium, the acting in conjunction by high temperature and high pressure promotes the densification of material, shortcoming is: apply pressure by gas or liquid to workpiece, the pressure of described gas or liquid is that isotropy is equal, but described gas or liquid act on the surface of workpiece by identical pressure, along with the change of Workpiece structure and thickness, inside workpiece everywhere, the pressure that the place of different structure shape is experienced is diverse, workpiece surface receives identical pressure effect in other words, but at inside workpiece or different depths, the inside that the identical pressure in surface produces or microcosmic pressure are diverse, so simple hot isostatic pressing, at identical external pressure and the sintering under identical external thermal effect, the heterogencity of sintered compact interior microscopic form will inevitably be caused, also will cause the defect on ceramic material property.
Discharge plasma sintering is a kind of type material process of preparing that development in recent years is got up.Be otherwise known as pulse electric current sintering.The principal feature of this technology utilizes body to heat and surface active, realizes the supper-fast densification sintering of material; Shortcoming is: it is uneven that the product after sintering there will be performance profile along current electric fields direction, because the distribution of electric field magnetic line of force can produce Territorial Difference to stupalith; Utilize microcosmic heating plasma, microtexture lacks pressure effect; The electric discharge applied or pulsed current have strong directivity or polarity, can form current channel or dodge road phenomenon, make the homogeneity of integral sintered body microtexture bad, cause sintered compact overall performance difference or directional difference in base substrate.
Chinese patent CN1478757A, discloses a kind of method that discharge plasma sintering prepares high-purity block titanium alumina-carbon material; Patent CN1817434A, discloses a kind of method of spark plasma sintering crystallization cubic boron nitride sintered body; Be all utilize discharge plasma sintering technique, apply plasma pulse electric current in the axis of base substrate, the Gradient distribution difference of microcosmic can be produced like this to the internal performance of sintered compact.
Chinese patent CN103343249A, disclose a kind of preparation method of electric field driven in-situ gradient thermoelectric material, the method utilizes directed resistance sintering to prepare grade thermoelectric material, make thermoelectric material under the effect in electric field and temperature field, the inner particles of material forms directional gradient distribution.
In sum, existing sintering method, the applying of pressure and transmission, heat generation with transmit the effect all well not realizing the isotropy uniformity of whole workpiece sintering body, so the stupalith that sinters out, the properties of Macrocosm and microcosm can exist defect in various degree certainly; The space that still there is technology improvement is controlled in the directivity of pressure, heat energy.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method, being called for short the field control sintering such as two, ceramic sintering technology is combined with electric field controls technology, hot isostatic pressing and discharge plasma sintering technique are merged mutually, and the electromagnetic field control techniques of innovative design plasma discharging process and method, thus improve pressure applying and transmission in existing sintering technology, heat energy produces the defect with transmission, make the pressure of both macro and micro, temperature, electric field is in controlled change, formation microcosmic is truly respectively to homogeneity, control and given play to isostatic pressed, put ionic discharge, electromagnetic field controls the advantage of sintering, under electromagnetic field controls, horizontal deflection and movement are flow to plasma discharging, thus the successful sintering of implementation structure pottery, obtain quality structure stupalith.
The present invention needs the gordian technique point solved, that isostatic pressing technology is combined with discharge plasma sintering technique, and use electromagnetic field control techniques to carry out field control and skew to the pulsed current in discharge plasma sintering, overcome the deficiency of discharge plasma sintering, omnibearing stereo formula is burnt thoroughly, crystal boundary and dot matrix, Macrocosm and microcosm acting in conjunction, implementation structure forming process of ceramics and sintering technology new development.
For achieving the above object, technical scheme of the present invention is as follows: a kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method, comprise ceramic body preparation, the field such as two control sintering oven, ceramic sintered bodies processing, the field control sintering method such as two, it is characterized in that:
Described ceramic body preparation, comprises raw and auxiliary material, proportioning components, blank preparation, blank mixing, powder preparation, powder grinding, powder mixing and compression molding; Described raw and auxiliary material is the mixture of one or more in natural mineral powder, oxide powder, carbide powder or nitride powder, and auxiliary agent: properties-correcting agent, lubricant, fluidizer etc., described additive is MgO, Y
2o
3, La
2o
3, ZrO
2in one, or any two mixture wherein, or any three kinds of mixtures wherein; Described additive addition is 0.01%---0.5%.
Prepare according to proportioning components; The raw material prepared is carried out preliminary ground and mixed, high-pressure homogeneous after, to dust granulation through spray tower, powder after granulation of dusting, through three-dimensional hybrid shredder ground and mixed, obtain uniform ceramic material powder, ceramic material powder is loaded in the mould of component to be processed, through shaped by fluid pressure, obtains the blank of compression molding.
Describedly two wait that field control sintering oven comprises lower furnace body, thermopair, upper furnace body, battery lead plate, bench insulator, contact conductor, graphite packing, workpiece, cooling water outlet, control electric field, rubber sealing boot, insulation ring seat, tensimeter, gas cylinder, air valve, compressor, gas inlet and outlet, impulse current generator, sintering controller, cold water inlet, fixed feet, electric field go between and tongued and grooved flanges.
Described upper furnace body and lower furnace body form the field such as two by tongued and grooved flanges and control and sinter body of heater, and described body of heater is provided with cooling water sandwich, and lower furnace body side is provided with cold water inlet, and upper furnace body side is provided with cooling water outlet, for the regulating and control of furnace body temperature; Described upper furnace body side is provided with thermocouple probe, for carrying out Real-Time Monitoring to temperature in body of heater.Described body of heater inner top and bottom are respectively arranged with bench insulator, described bench insulator is provided with battery lead plate, described battery lead plate is connected with body of heater external pulse current generator by contact conductor, produces pulsed current by impulse current generator, and then carries out discharge plasma sintering to workpiece; Described battery lead plate is upper and lower two pieces, between described upper and lower two electrode plate, be provided with rubber sealing boot, in described rubber sealing boot, be filled with graphite packing, the effect of fixing internal workpiece and On current is played in described graphite packing, and described graphite packing center is mounted with workpiece to be sintered;
Described lower furnace body inside is provided with multiple control electric field, described control electric field is flat structure, polylith controls electric fields uniform and is circular layout in the middle part of body of heater, described control electric field is by the dead ring seat supports bottom it, described insulation ring seat is supported by multiple fixed feet, described fixed feet is fixedly welded on inboard wall of furnace body, described insulation ring seat and fixed feet are welded and fixed, described insulation ring seat and fixed feet are provided with inner sleeve, for the electric field lead-in wire controlling electric field is drawn outside body of heater, and be connected with sintering controller; Described workpiece to be sintered, is embedded in the middle of graphite packing.
Described body of heater is sealed high-voltage resistant structure, gas inlet and outlet is provided with bottom it, described gas inlet and outlet, be connected with compressor and gas cylinder respectively, between described gas inlet and outlet and compressor, gas cylinder, be provided with tensimeter and air valve, described air valve is for controlling switch or the relief pressure of gas conveying; When gas is passed in body of heater, namely furnace interior produces high pressure, and the rubber seal that described high pressure puts in stove puts, and then is put on by pressure on graphite packing and workpiece to be sintered.
Described body of heater is outside equipped with impulse current generator and sintering controller, described contact conductor, electric field lead-in wire, thermopair are all communicated with sintering controller, described impulse current generator is communicated with electrode outlet line, by sintering controller, sintering process process is controlled, realize the two of stupalith base substrate and wait field control to sinter.
Described ceramic sintered bodies processing, comprises the demoulding of sintered compact blank, blank shaping, roughing, precision work, component polishing and component finished product; Ceramic body is in the field control sintering oven such as two after sintering, namely workpiece becomes sintered compact, sintered compact is taken out from the field control sintering oven such as two, again utilize after graphite packing collection and treatment, the sintered compact demoulding and shaping, the workpiece of sintering is carried out roughing and precision work by technological standards requirement, then carries out lapping and polishing, namely obtain component finished product.
Described twoly wait field to control sintering method to be: ceramic powder loads in rubber cuff or ceramic part is imbedded in powdered graphite; Load the field control sintering ovens such as two, pass into protective gas and apply isostatic pressure, according to different stupaliths, the gaseous tension applied is 10---100MPa; According to the actual requirement of material, applying pulse plasma electric current, is 70 DEG C according to temperature rise rate---700 DEG C/min, and the temperature parameter of the field control sintering ovens such as control is two; Adjustment simultaneously controls the intensity of electric field with control annular and alternately changes, along with the rising of in-furnace temperature, the intensity of voltage stabilizing pulsed current can improve gradually, and the intensity of described control electric field also increases, and guarantees that the effect of peripheral electric field to base substrate interior plasma state material is in significant condition; When the temperature in sintering oven reaches sintering temperature, common sintering temperature region is 1000 DEG C---2000 DEG C; Keep temperature 1min---25min; According to temperature conditions in sintering oven, by increasing pulsed current, increasing peripheral control strength of electric field, or cooling process is carried out to sintering oven, control the temperature variation in sintering process; After being incubated, close impulse current generator switch, closing control electric field switch, twoly wait field control sintering oven naturally cooling or cooled by cooling sandwith layer, after system is lowered the temperature, release; From the field control sintering oven such as two, take out sintered compact, carry out roughing and precision work.
The stupalith that the present invention sinters, bending strength or reach 500---900MPa; Fracture toughness property can reach 5---10MPam
1/2; Density can reach more than 99.0; Vickers' hardness can reach 20---50GPa.
Operating process of the present invention is: according to working specification, workpiece to be sintered is loaded two field of waiting and control in sintering oven, furnace sealing is adjusted parameters to original state, connect and control power supply, check whole sintering system, open source of the gas, open compressor and control air valve, pressure is applied to furnace interior, when furnace pressure reaches preset pressure, open impulse current generator, load electric current is progressively added to power-on and power-off pole plate, voltage stabilizing pulsed current is by graphite district, and act on base substrate to be sintered, because pulsed current causes base substrate inside that plasma discharging occurs, and rapid temperature increases, after reaching sintering temperature, inside workpiece and outside all obtain pulse current discharging effect, produce isostatic pressed External Force Acting and the effect of pulsed current internal discharge, while sintering, sintering controller controls many groups electric field of annular spread, pulsed is applied to workpiece, the electric field action of alternation, by the impact of pulse alternating electric field, cause pulsed current and the electromagnetic field environment of inside workpiece, the power change of following external electrical field changes with direction of an electric field, synchronously carry out multi-angle in real time, multi-direction change, thus realize between inside workpiece lattice, between crystal boundary, between melt body, molten between matter and solvent, between solid phase and liquid phase, complicated exchange and fusion is there is between gas phase and liquid phase, and the specific surface area between ceramic particle and internal energy are fully optimized, thus obtain high quality high performance structural stupalith.
Described two field control sintering method that waits is at body of ceramic material inside Omnidirectional heating, overall surface activation is carried out at the Macrocosm and microcosm of material, in inner phase change, lattice variations, crystal boundary changes and draws in gas process, the whole mode of action is three-dimensional, multi-direction, carry out at many levels, therefore direction and changes of magnetic field effect is applied at electric field, heat energy produces and propagates, impressed pressure is with under inner moment plasma discharge pressure acting in conjunction, the general effect embodied is exactly in sintering process, Macrocosm and microcosm each to homogeneity and consistence, thus make sintered compact obtain excellent ceramic material property performance, and the performance of the stupalith obtained performance uniformity in all directions.
Describedly two the mechanism that sintering method is controlled in field is waited to be: solid state sintering and liquid phase sintering are also deposited, microcosmic plasma discharge produces moment microexplosion and plasma gas phase, so in whole sintering process, solid phase under microstate, liquid phase, gas phase depositing, under electric field and magnetic field alternation effect, under outside isostatic pressed and inner microexplosion pressure, uniform thermal energy transfer makes the ceramic lattice under microstate, crystal boundary, surface, interface all Rapid Variable Design occur.Under microstate, solid-state, liquid, gaseous state and the comprehensive action of plasma state material, reciprocal effect, microexplosion, micro-sudden strain of a muscle, micro-melting betide multi-direction, achieve heat energy and produce and the homogenizing transmitted, electric field and magnetic field discharge homogenizing, the rearrangement restructuring homogenizing of microcosmic ceramic particle.
Described control electric field is at least set to two, and symmetrical annular is arranged in the periphery of workpiece to be sintered, the electric field that symmetry is circular layout, constitute the three-dimensional induction areas of impact workpiece to be sintered, huge effect is produced for upper/lower electrode plasma discharging pulsed current, and there is synchronous displacement, this multidirectional pulsed current displacement along with the alternation in exterior annular stereoscopic electric magnetic field, in microtexture, create the reactive force of multi-C stereo; Under the control of sintering controller, controlling electric field can change intensity, and also may change direction of an electric field, more can change the symmetrical form of electric field, this diverse external electric field influence mode is the reason that stupalith well sinters.
Usual gas or liqu id plasmas are in-between the electrodes, make medium-gas or liquid, as nitrogen or air etc. by high current intensity, be ionized into negatively charged ion and positively charged ion, plasma inside is the aggregate of zwitterion, and totally keeps electric neutrality, is called plasma body; Described plasma body along the electric field formed between electrode, i.e. flux regions distribution; In Conventional plasma sintering, be that electric field electrode is arranged at stupalith both sides, and make electrode directly with material to be sintered, guarantee current lead-through; During sintering, electrode applies big current intensity, convey electrical current in ceramic body to be sintered by electrode, when strong current is by ceramic body to be sintered, by the conducting material in ceramic body in solid-state crystal boundary and microcosmic dot matrix region, be dissociated into isoionic state, and produce high temperature.
Action principle of the present invention: in micro, electric discharge makes microcosmic particle produce plasma state, and occurs the microcosmic plasma clustering collective of High Temperature High Pressure; Under pulsed current and additional electromagnetic field effect, microcosmic plasma body is moved, be out of shape, microexplosion, micro-sudden strain of a muscle etc.; Microcosmic plasma body moving, be out of shape, microexplosion and micro-ly flash in journey, electron opaque material is had an immense impact on, thermal energy transmits fast, high field polarization is torn, high pressure, high temperature and high magnetic field intensity; After the field control conversion of moment, the migration of the melt of microcosmic local, decompression, cooling, make system towards more stable condition conversion; Macroscopic field control makes microcosmic plasma body generation remotely migrating, the population equilibrium of increase system, microcosmic plasma body is subject to the restriction of microcosmic crystal boundary and dot matrix, microexplosion, micro-sudden strain of a muscle and field control effect, microcosmic plasma body can be forced to break through the potential energy barrier of crystal boundary and dot matrix, thus obtain the excellent sintering of ultra-hard abrasive material, greatly improve the property indices of ultra-hard abrasive material.
The mechanism of field of the present invention control techniques: owing to employing electric field controls technology, in original sintering process, outside plasma electrode, be provided with control electric field, in plasma agglomeration process, by extra electric field, electric field influence effect is applied to solid fraction state plasma body, the plasma body produced during sintering, at originally fixing grain boundary area and dot matrix region isoionic state particle, will offset, vibrate, recombinate; The change of the skew that this solid state plasma occurs under DC Electric Field, vibration, restructuring, region is stereo directional occurs, skew is subject to the restriction of electric field strength with the amount of vibration, and the action direction that skew is also subject to extra electric field with the direction of vibration affects; Restructuring change is then relevant with dot matrix microenvironment to the crystal boundary of solid state plasma, the component of the temperature in micro, adjacent grain boundary and dot matrix, the kind of non-electric conductivity particle are all relevant with character, and final result is: under the effect of external electric field, the skew that solid state plasma occurs, vibration and restructuring, accelerate the speed of plasma agglomeration stupalith, improve the quality of plasma agglomeration stupalith, improve the properties of plasma agglomeration stupalith, add the hardness of stupalith, wear resistance, preservative property etc.
The combination of isostatic pressing technology of the present invention and plasma sintering technique, not only when stupalith sinters, produce the change of the plasma body of microtexture and the micro-skew of various microcosmic, vibration, restructuring, but also can in isostatic pressed mode, huge pressure is applied at macroscopically plasma, by the hydrostatic pressure of macroscopic view, the pressure action high to the plasma generation of solid-state lower microcosmic liquefaction, makes stupalith to be sintered be subject to the impact of another reactive force.
The feature of overall technical architecture of the present invention is: (1) microcosmic plasma body instantaneous high-temperature, and by high temperature transferring heat energy radiation towards periphery, affects non-conductometric particle, forms moment melting partial liquid phase region; (2) under the effect of microcosmic local plasma, form localized liquid stupalith region, it is the body region of microcosmic plasma body, due to the formation in partial liquid phase region, change the solid-state balance of microcosmic regional area, and by partial liquid phase region, adjacent solid matter is exerted one's influence, improve the bonding tightness of stupalith; (3) microcosmic crystal boundary and dot matrix are under External Electrical Field, and the skew of crystal boundary and dot matrix, vibration, restructuring occur, and are stupalith sintering and shaping key; (4) change direction of extra electric field and change frequency effect, make above-mentioned each factor solid-state with on the stereo directional of partial liquid phase stupalith, constantly carry out changing and break through, and at each independently between regional area, formation punctures, micro-sudden strain of a muscle, microexplosion, electric discharge, resonance etc. micro-variations, bulk ceramics material is had on solid space homogenized, and directly have influence on neighbouring Non-conductive particles, be that stupalith can combine and form the important factor of superhard wear high performance material between different component; (5) the hydrostatic pressure effect of macroscopic view, make the outside isostatic pressure effect waiting sintered ceramic material to be continued, and the partial liquid phase region in solid ceramic material is had an impact, skew, the vibration of localized region, recombinate and puncture, micro-sudden strain of a muscle, microexplosion, electric discharge, the electrical phenomena such as resonance all produce more effective promoter action, lasting isostatic pressure is constantly change or the stupalith regional area occurred instantaneously, microcosmic, submicroscopic region provide the propulsion source tightened with tight clusters; (6) controlled external electric field, in the peripheral distribution mode of strength of electric field, direction of an electric field, electric field change frequency, electric field, all controllable, directly have influence on the change of stupalith Macrocosm and microcosm structure, to transmission, the crystal boundary of the transmission of isostatic pressed, high temperature heat and dot matrix is broken through, the generation of micro-sudden strain of a muscle microexplosion, offset the direction vibrated and recombinate and all serve crucial effect; (7) the field control techniques of gas or liquid isostatic pressed and extra electric field acts on stupalith to be sintered, but not affecting the body of stupalith, solid-state under microstate, liquid, gaseous state and plasma state coexist, and electric field magnetic field interacts, comprehensive action is also one of feature of the present invention.
Pass through technique scheme, the beneficial effect of technical solution of the present invention is: isostatic pressed three dimensional field control discharge plasma sintering is plasma state based on material itself and generates heat, be essentially different with by the type of heating of external heat source, the energy mode that polarizes, luminous energy mode, plasma discharging is compared with conventional energy presentation mode has obvious advantage and feature, as high in efficiency, capacity usage ratio is high, pollution-free, can overall rapid heating, sintering temperature reduce, the uniform microstructure etc. of material.(1) heating and sintering velocity are exceedingly fast.The traditional heating of material reaches homogeneous temperature by sample conduction from outward appearance to inner essence.Due to the poor thermal conductivity of most stupalith, therefore heating and sintered ceramic need for a long time, generally in hour, large component institute's time spent is just longer.Two sintering such as grade is that material internal entirety heats simultaneously, heat-up rate is fast, thus substantially reduce sintering time, particularly to the sintering of some stupaliths, from being reduced in several days even several weeks by two several minutes magnitudes waiting sintering of past, thus drastically increase the utilization ratio of production efficiency and the energy.(2) instantaneity and pollution-free.Due to not through thermal conduction in the sintering process such as two, thus there is no thermal inertia, namely there is instantaneity, can instantaneous break thermal source and heating in time, embody energy-conservation and be easy to the feature that controls.Meanwhile, the sintering such as two can not pollute sintered material, can be conveniently implemented in the sintering under vacuum and various atmosphere and pressure, also can not produce obnoxious flavour contaminate environment as oil firing, gas, coal etc. in sintering process.(3) energy-efficient.The sintering temperature such as two is compared with nominal sintering temperatures, and maximum cooling extent can reach about 500; The efficiency being generally transformed into heat energy from plasma energy can reach more than 90%, in addition twoly waits the time of sintering short, therefore greatly can reduce energy consumption.(4) selective sintering.For heterogeneous mixing material, due to the difference of different media plasma ability, the equivalent ionic strength of generation is different, and heat effect is also different, utilizes this point can carry out selective sintering to matrix material.(5) microstructure and the macro property of stupalith is improved.Because the speed of two sintering such as grade is fast, the time is short, thus avoids the abnormal growth of crystal grain in sintering process, finally can obtain the superfine crystal particle structural ceramic material with high strength and toughness.(6) shapingly can realize a step complete with sintering, gas-static regulates and controls with external electric field and plasma agglomeration combines, and makes the shaping of ceramic structure material can realize a step with sintering and completes, improve efficiency, save cost, closed product performance and obtain tremendous increase.(7) the present invention makes the shaping of stupalith shorten process time and cycle with sintering, thus can output in enormous quantities, raises labour efficiency, the competitive power of increase enterprise.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can be obtained according to these accompanying drawings.
Fig. 1 is a kind of stupalith sintering oven disclosed in the embodiment of the present invention and isostatic pressed field control plasma agglomeration method structural representation;
Fig. 2 is a kind of stupalith sintering oven disclosed in the embodiment of the present invention and isostatic pressed field control plasma agglomeration method A-A sectional view schematic diagram;
Fig. 3 is a kind of stupalith sintering oven disclosed in the embodiment of the present invention and isostatic pressed field control plasma agglomeration method process flow diagram;
Fig. 4 is a kind of stupalith sintering oven disclosed in the embodiment of the present invention and isostatic pressed field control plasma agglomeration method technical process mark figure;
Fig. 5 is a kind of stupalith sintering oven electric field structure schematic diagram disclosed in the embodiment of the present invention 2;
Fig. 6 is a kind of stupalith sintering oven electric field structure schematic diagram disclosed in the embodiment of the present invention 3.
Numeral and the corresponding component title represented by letter in figure:
1. 4. blank mixing prepared by raw and auxiliary material 2. proportioning components 3. blank
5. powder is prepared 6. powders and is ground 7. powders and mix 8. compression moldings
9. the field control sintering 10. blank demoulding 11. blank shaping 12. roughing such as pair
13. precision work 14. component polishing 15. component finished product 16. lower furnace bodies
17. thermopair 18. upper furnace body 19. battery lead plate 20. bench insulators
21. contact conductor 22. graphite packing 23. workpiece 24. cooling water outlets
25. control electric field 26. rubber sealing boots 27. insulate ring seat 28. tensimeter
29. gas cylinder 30. air valve 31. compressor 32. gas inlet and outlets
33. impulse current generators 34. sinter controller 35. cold water inlet 36. fixed feet
37. electric fields go between 38. tongued and grooved flanges
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
According to Fig. 1, Fig. 2, Fig. 3 and Fig. 4, the invention provides a kind of stupalith sintering oven and isostatic pressed field control plasma agglomeration method, comprise ceramic body preparation, the field control sintering oven such as two, ceramic sintered bodies processing, the field control sintering method such as two, it is characterized in that:
Described ceramic body preparation, comprise raw and auxiliary material 1, proportioning components 2, blank preparation 3, blank mixing 4, powder prepare 5, powder grinding 6, powder mixing 7 and compression molding 8; Described raw and auxiliary material 1 is the mixture of one or more in natural mineral powder, oxide powder, carbide powder or nitride powder, and auxiliary agent: properties-correcting agent, lubricant, fluidizer etc., prepares according to proportioning components 2;
Preferably, described additive is: ZrO
2, adding per-cent is 0.25%;
The raw material prepared is carried out preliminary powder grinding 6 mixing, high-pressure homogeneous after, to dust preparation 5 granulation through spray tower, powder after granulation of dusting, 6 machine ground and mixed are ground through three-dimensional hybrid powder, obtain uniform ceramic material powder, ceramic material powder is loaded in the mould of component to be processed, through shaped by fluid pressure, obtains the blank of compression molding 8.
Describedly two wait field control sintering oven to comprise lower furnace body 16, thermopair 17, upper furnace body 18, battery lead plate 19, bench insulator 20, contact conductor 21, graphite packing 22, workpiece 23, cooling water outlet 24, control electric field 25, rubber sealing boot 26, insulation ring seat 27, tensimeter 28, gas cylinder 29, air valve 30, compressor 31, gas inlet and outlet 32, impulse current generator 33, sintering controller 34, cold water inlet 35, fixed feet 36, electric field go between 37 and tongued and grooved flanges 38; It is characterized in that:
Described upper furnace body 18 and lower furnace body 26 form the field such as two by tongued and grooved flanges 38 and control and sinter body of heater, described body of heater is provided with cooling water sandwich, lower furnace body 16 side is provided with cold water inlet 35, and upper furnace body 18 side is provided with cooling water outlet 24, for the regulating and control of furnace body temperature; Described upper furnace body 18 side is provided with thermopair 17 and pops one's head in, for carrying out Real-Time Monitoring to temperature in body of heater.Described body of heater inner top and bottom are respectively arranged with bench insulator 20, described bench insulator is provided with battery lead plate 19, described battery lead plate 19 is connected with body of heater external pulse current generator 33 by contact conductor 21, produce pulsed current by impulse current generator 33, and then discharge plasma sintering is carried out to workpiece 23; Described battery lead plate 19 is upper and lower two pieces, between described upper and lower two electrode plate 19, be provided with rubber sealing boot 26, graphite packing 22 is filled with in described rubber sealing boot 26, the effect of fixing internal workpiece 23 and On current is played in described graphite packing 22, and described graphite packing 22 center is equipped with workpiece 23 to be sintered.
Described lower furnace body 16 inside is provided with multiple control electric field 25, described control electric field 25 is flat structure, polylith controls the even annular of electric field 25 and is arranged in the middle part of body of heater, described control electric field 25 is supported by the insulation ring seat 27 bottom it, described insulation ring seat 27 is supported by multiple fixed feet 36, described fixed feet 36 is fixedly welded on lower furnace body 16 inwall, described insulation ring seat 27 is welded and fixed with fixed feet 36, described insulation ring seat 27 and fixed feet 36 are provided with inner sleeve, for the electric field lead-in wire 37 controlling electric field 25 is drawn outside lower furnace body 16, and be connected with sintering controller 34, described workpiece to be sintered 23, is embedded in the middle of graphite packing 22.
Described body of heater is sealed high-voltage resistant structure, gas inlet and outlet 32 is provided with bottom it, described gas inlet and outlet 32 is connected with compressor 31 and gas cylinder 29 respectively, between described gas inlet and outlet 32 and compressor 31, gas cylinder 29, be provided with tensimeter 28 and air valve 30, described air valve 30 is for controlling switch or the relief pressure of gas conveying; When gas is passed in body of heater, namely furnace interior produces high pressure, and described high pressure puts on the rubber sealing boot 26 in stove, and then is put on by pressure on graphite packing 22 and workpiece to be sintered 23.
Described body of heater is outside equipped with impulse current generator 33 and sintering controller 34, described contact conductor 37, electric field lead-in wire 21, thermopair 17 are all communicated with sintering controller 34, described impulse current generator 33 and electrode are drawn 37 lines and are communicated with, controlled by sintering controller 34 pairs of sintering process processes, sintering 9 is controlled in the two fields of waiting realizing stupalith base substrate.
Described ceramic sintered bodies processing, comprises the sintered compact blank demoulding 10, blank shaping 11, roughing 12, precision work 13, component polishing 14 and component finished product 15; Ceramic body is in the field control sintering oven 9 such as two after sintering, namely workpiece 23 becomes sintered compact, sintered compact is taken out from the field control sintering oven 9 such as two, again utilize after graphite packing 22 collection and treatment, the sintered compact demoulding and shaping, the workpiece of sintering is carried out roughing 12 and precision work 13 by technological standards requirement, then carries out lapping and polishing, namely obtain component finished product 15.
Sintering method is controlled for load in rubber cuff by alumina ceramic powder in described two field of waiting; Load the field control sintering ovens such as two, pass into protectiveness nitrogen and apply isostatic pressure, the gaseous tension applied is 15---30MPa; According to the actual requirement of material, applying pulse plasma electric current, is 500 DEG C according to temperature rise rate---700 DEG C/min, the temperature parameter of the field control sintering ovens such as control is two is 1100 DEG C---and 1450 DEG C; Adjustment simultaneously controls the intensity of electric field with control annular and alternately changes, along with the rising of in-furnace temperature, the intensity of voltage stabilizing pulsed current can improve gradually, and the intensity of described control electric field also increases, and guarantees that the effect of peripheral electric field to base substrate interior plasma state material is in significant condition; When the temperature in sintering oven reaches sintering temperature, keep temperature 10min; According to the temperature conditions in sintering oven, by increasing pulsed current, increasing peripheral control strength of electric field, or cooling process is carried out to sintering oven, control the change of temperature in sintering process; After being incubated, close impulse current generator switch, closing control electric field switch, twoly wait field control sintering oven naturally cooling or cooled by cooling sandwith layer, after system is lowered the temperature, release; From the field control sintering oven such as two, take out sintered compact, carry out roughing and precision work.
The stupalith that the present invention sinters, bending strength or reach 700MPa; Fracture toughness property can reach 8MPam
1/2; Density can reach more than 99.5; Vickers' hardness can reach 40GPa.
Operating process of the present invention is: according to working specification, workpiece to be sintered is loaded two field of waiting and control in sintering oven 9, furnace sealing is adjusted parameters to original state, connect and control power supply, check whole sintering system, open gas cylinder 29, open compressor 31 and control air valve 30, pressure is applied to furnace interior, when furnace pressure reaches preset pressure, open impulse current generator 33, load electric current is progressively added to power-on and power-off pole plate 19, pulsed current is by graphite packing 22 district, and act on base substrate to be sintered, because pulsed current causes base substrate inside that plasma discharging occurs, and rapid temperature increases, after reaching sintering temperature, workpiece 23 is inner all obtains pulse current discharging effect with outside, produce isostatic pressed External Force Acting and the effect of pulsed current internal discharge, while sintering, sintering controller 34 controls many groups electric field 25 of annular spread, pulsed is applied to workpiece 23, the electric field action of alternation, by the impact of pulse alternating electric field 25, cause pulsed current and the electromagnetic field environment of workpiece 23 inside, the power change of following external electrical field 25 changes with direction of an electric field, synchronously carry out multi-angle in real time, multi-direction change, thus realize between workpiece 23 internal crystal framework, between crystal boundary, between melt body, molten between matter and solvent, between solid phase and liquid phase, complicated exchange and fusion is there is between gas phase and liquid phase, and the surface-area between ceramic particle and internal energy are fully optimized, thus obtain high quality high performance structural stupalith.
Embodiment 1, the field control sintering ovens such as uniform six control electric fields are two; As shown in Figure 2;
Embodiment 2, the field control sintering ovens such as uniform four control electric fields are two; As shown in Figure 5;
Embodiment 3, the field control sintering ovens such as uniform three arcs control electric field is two; As shown in Figure 6;
Stupalith isostatic pressed field of the present invention control discharge plasma sintering is plasma state based on material itself and generates heat, be essentially different with by the type of heating of external heat source, the energy mode that polarizes, luminous energy mode, plasma discharging is compared with conventional energy presentation mode has obvious advantage and feature, as high in efficiency, capacity usage ratio is high, pollution-free, can overall rapid heating, sintering temperature reduce, the uniform microstructure etc. of material.(1) heating and sintering velocity are exceedingly fast.The traditional heating of material reaches homogeneous temperature by sample conduction from outward appearance to inner essence.Due to the poor thermal conductivity of most stupalith, therefore heating and sintered ceramic need for a long time, generally in hour, large component institute's time spent is just longer.Two sintering such as grade is that material internal entirety heats simultaneously, heat-up rate is fast, thus substantially reduce sintering time, particularly to the sintering of some stupaliths, from being reduced in several days even several weeks by two several minutes magnitudes waiting sintering of past, thus drastically increase the utilization ratio of production efficiency and the energy.(2) instantaneity and pollution-free.Due to not through thermal conduction in the sintering process such as two, thus there is no thermal inertia, namely there is instantaneity, can instantaneous break thermal source and heating in time, embody energy-conservation and be easy to the feature that controls.Meanwhile, the sintering such as two can not pollute sintered material, can be conveniently implemented in the sintering under vacuum and various atmosphere and pressure, also can not produce obnoxious flavour contaminate environment as oil firing, gas, coal etc. in sintering process.(3) energy-efficient.The sintering temperature such as two is compared with nominal sintering temperatures, and maximum cooling extent can reach about 500; The efficiency being generally transformed into heat energy from plasma energy can reach more than 90%, in addition twoly waits the time of sintering short, therefore greatly can reduce energy consumption.(4) selective sintering.For heterogeneous mixing material, due to the difference of different media plasma ability, the equivalent ionic strength of generation is different, and heat effect is also different, utilizes this point can carry out selective sintering to matrix material.(5) microstructure and the macro property of stupalith is improved.Because the speed of two sintering such as grade is fast, the time is short, thus avoids the abnormal growth of crystal grain in sintering process, finally can obtain the superfine crystal particle structural ceramic material with high strength and toughness.(6) shapingly can realize a step complete with sintering, gas-static regulates and controls with external electric field and plasma agglomeration combines, and makes the shaping of ceramic structure material can realize a step with sintering and completes, improve efficiency, save cost, closed product performance and obtain tremendous increase.(7) the present invention makes the shaping of stupalith shorten process time and cycle with sintering, thus can output in enormous quantities, raises labour efficiency, increase enterprise competitiveness.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (5)
1. a stupalith sintering oven, is called for short the field control sintering ovens such as two; It is characterized in that, comprise lower furnace body, thermopair, upper furnace body, battery lead plate, bench insulator, contact conductor, graphite packing, workpiece, cooling water outlet, control electric field, rubber sealing boot, insulation ring seat, tensimeter, gas cylinder, air valve, compressor, gas inlet and outlet, impulse current generator, sintering controller, cold water inlet, fixed feet, electric field lead-in wire and tongued and grooved flanges; Described upper furnace body and lower furnace body form by tongued and grooved flanges the body of heater that sintering oven is controlled in the field such as two, and described body of heater is provided with cooling water sandwich and water coolant gangway; Described upper furnace body side is provided with thermocouple probe, and described body of heater inner top and bottom are respectively arranged with bench insulator, and described bench insulator is provided with battery lead plate, and described battery lead plate is connected with body of heater external pulse current generator by contact conductor; Described battery lead plate is upper and lower two pieces, between described upper and lower two electrode plate, be provided with rubber sealing boot, in described rubber sealing boot, be filled with graphite packing, the effect of fixing internal workpiece and On current is played in described graphite packing, and described graphite packing center is mounted with workpiece to be sintered.
2. a kind of stupalith sintering oven according to claim 1, it is characterized in that, described lower furnace body inside is provided with multiple control electric field, described control electric field is flat structure, polylith controls electric fields uniform and is circular layout in the middle part of body of heater, described control electric field is by the dead ring seat supports bottom it, described insulation ring seat is supported by multiple fixed feet, described fixed feet is fixedly welded on inboard wall of furnace body, described insulation ring seat and fixed feet are welded and fixed, described insulation ring seat and fixed feet are provided with inner sleeve, for the electric field lead-in wire controlling electric field is drawn outside body of heater, and be connected with sintering controller, described workpiece, is embedded in the middle of graphite packing.
3. a kind of stupalith sintering oven according to claim 1, it is characterized in that, described body of heater is sealed high-voltage resistant structure, gas inlet and outlet is provided with bottom it, described gas inlet and outlet, be connected with compressor and gas cylinder respectively, between described gas inlet and outlet and compressor, gas cylinder, be provided with tensimeter and air valve.
4. field control sintering such as utilizing stupalith sintering oven as claimed in claim 1 to carry out a method for stupalith isostatic pressed field control plasma agglomeration, it is characterized in that, comprise ceramic body preparation, ceramic sintered bodies is processed, be two; Described ceramic body preparation, comprises the preparation of raw and auxiliary material component, blank preparation, blank mixing, powder preparation, powder grinding, powder mixing and compression molding; Described ceramic sintered bodies processing, comprises the demoulding of sintered compact blank, blank shaping, roughing, precision work, component polishing and component finished product; Describedly two field control is waited to be sintered to: carry out plasma pulse electric current sintering by power-on and power-off pole plate to workpiece, by being arranged on the control electric field of surrounding, applying electromagnetic action, applies isostatic pressure by environmental gas to workpiece; Impulsive discharge, electromagnetic control and additional isostatic pressed comprehensive action, sintered ceramic base substrate.
5. the method for a kind of stupalith isostatic pressed field control plasma agglomeration according to claim 4, it is characterized in that, described control electric field is at least set to two, is arranged symmetrically with; Described control electric field annular is arranged in the middle part of body of heater; Described control electric field is in sintering process, and strength of electric field, direction of an electric field be change alternately, the pulsed current of influence in workpiece, thus changes lattice, crystal boundary, dot matrix micro and the structure in stupalith; Synchronously carry out multi-angle, multi-direction change in real time, thus to realize between inside workpiece lattice, between crystal boundary, between melt body, molten between matter and solvent, between solid phase and liquid phase, occur between gas phase and liquid phase to exchange and merge.
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| CN107216153A (en) * | 2017-06-27 | 2017-09-29 | 广东工业大学 | A kind of 3D printing method of ceramic material |
| CN108468025B (en) * | 2018-02-11 | 2023-08-22 | 东莞市欧莱溅射靶材有限公司 | Hot isostatic pressing treatment method for chromium planar target material |
| CN111024462A (en) * | 2018-10-09 | 2020-04-17 | 中国科学院金属研究所 | Sample design and experiment method for realizing high hydrostatic pressure and accurate temperature measurement and control |
| CN111423224A (en) * | 2020-04-17 | 2020-07-17 | 汪平南 | Red interior line ceramic material, ceramic product, preparation method and application thereof |
| CN113154882B (en) * | 2021-04-27 | 2023-08-29 | 华南师范大学 | Pressureless rapid sintering device and sintering method for 3D printing |
| CN114369739B (en) * | 2021-12-14 | 2022-08-26 | 江西理工大学 | Preparation method and device of lead-free graphite brass composite material |
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