CN102601361B - Split high-temperature preheating powder explosive sintering device - Google Patents

Split high-temperature preheating powder explosive sintering device Download PDF

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CN102601361B
CN102601361B CN2012100962661A CN201210096266A CN102601361B CN 102601361 B CN102601361 B CN 102601361B CN 2012100962661 A CN2012100962661 A CN 2012100962661A CN 201210096266 A CN201210096266 A CN 201210096266A CN 102601361 B CN102601361 B CN 102601361B
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assembly
shock wave
powder
temperature
explosive
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CN102601361A (en
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陈鹏万
周强
尹昊
高鑫
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Beijing Institute of Technology BIT
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Abstract

The invention discloses a split high-temperature preheating powder explosive sintering device, which comprises a shock wave loading component, a controllable split component and a sample high-temperature recovery component, wherein the shock wave loading component can be locked and released by the aid of the controllable split component. The explosion shock pressure and the continuous action time of shock waves can be precisely adjusted by means of adjusting experimental conditions, the highest preheating temperature of powder to be sintered can be higher than 1000 DEG C by means of a chemical heating method or an electric heating method, the optimal initiation time can be determined by means of making multiple experiments according to sintering conditions.

Description

Split type high temperature preheating powder explosive sintering device
Technical field
The present invention relates to high temperature preheating powder explosive sintering device, be specifically related to a kind of split type high temperature preheating powder explosive sintering device.
Background technology
Explosive sintering also claims explosive consolidation, is the shock wave that utilizes explosive charge or film flying to hit to produce during by metal or ceramic powders, makes between adjacent powder particles and produces bonding, thereby form the technology of compact block.This technology has fast molten fast cold property, and TRANSIENT HIGH TEMPERATURE high pressure and high-strain-rate characteristics, be the effective ways that prepare balance/unbalance state material, is applied to the fields such as nano structural material, non-crystalline material, superhard material and hard-to-sinter dusty material.
For refractory metal and ceramic powders such as W, Mo, Ti, natural characteristic due to its high-melting-point, high fragility, when adopting normal temperature explosive consolidation technique, in order to improve density, often adopt the method that improves surge, but, easily produce simultaneously serious crackle in the sample of preparation.Therefore, reducing under the shock wave pressure prerequisite, treating sintered powder and carry out high temperature preheating and can prepare refractory metal or the ceramic composite of high-compactness, flawless, function admirable.Pre-heating powder explosive sintering technology becomes the dominant direction of Recent study, being most widely used of the heating techniques such as wherein electrical heating, self propagating high temperature synthetic (SHS) reaction intensification.
1) electrical heating method
Electrical heating method is that the Joule heat that produces while utilizing electric current by the high resistance electric furnace heating wire is treated sintered powder and carried out the method for high temperature preheating.Gorobtsov and Roman combine shock wave with the green compact technology of being rapidly heated, adopt the refractory materials such as the fixed tungsten heavy alloy of high temperature explosive consolidation (HEC) technique.Powder in electric furnace after preheating, is opened heating furnace cover when detonator is installed, with explosive above guide rail slides into the container that fills pre-heating powder.Mobile powder was controlled in 20 seconds to the time of detonating charge.Test shows that the HEC method that adopts higher than the material recrystallization temperature can obtain the theoretical density pressed compact.The patent of Akashi etc. has disclosed a kind of explosive consolidation device with a plurality of sample boxs.This device and external heat furnace accretion are combined, and after heater raises the temperature of whole steel explosive consolidation device, explosive container are slided into remote initiation on consolidation device.The Japan Hokamoto of Kumamoto university etc. has developed a kind of high temperature preheating powder underwater blast wave cavity blasting consolidation device, the Mohaupt effect of this technique has improved maximum impact pressure, and its shock wave continuous action time is more much longer than the film flying of Sawaoka and Akashi loading explosive consolidation technique.Powder heats under the condition of protective atmosphere; after the powder preheating finishes; by two cylinders that are connected with the oil-gas converter, heating furnace is descended; the shock wave charging assembly is placed on the powder assembly thereupon; explosive detonated in the moment of its underpart contact pre-heating powder assembly, and this device is used to the explosive consolidation experiment of diamond dust and c-BN powder.The principle design that M.A.Meyers etc. application cylinder charger dose is uniform plane wave explosive consolidation device.The rectangle sample box left-right symmetry juxtaposition of this device, place metal caul therebetween and can fall into as absorbing catching of back wave.Two groups of film flyings are arranged symmetrically with the Energy Transfer of explosive to sample box., propagate under the sliding detonation wave direction at device top detonating charge with linear plane wave producer (arranging the triangle powder column of emptying aperture), clash on the metal caul of centre, avoided the destruction of sample box.When the blast pressure that requires was low, this device can be without film flying, and this moment, explosive directly contacted with sample box.This device also is applicable to the preheating explosive consolidation of difficult consolidated powder, and to improve the ductility of powder matrix, sample box in electric furnace after preheating, slips into along the guide plate on destructor top.
The advantage of electrical heating method is accurately to control preheat temperature, but electrical heating method generally needs external electric furnace, makes the whole system complex structure, and, because electrical heating method is longer heat time heating time, for the fine grain powder, easily cause grain growth and lose original character.
2) synthetic (SHS) exothermic heat of reaction heating of self propagating high temperature
Synthetic (SHS) exothermic heat of reaction heating of self propagating high temperature is namely utilized SHS exothermic heat of reaction system to treat sintered powder as thermal source to carry out high temperature preheating.No. 5996385 United States Patent (USP)s of Kecskes are in conjunction with the people's such as Niiler two-step method and the people's such as Takeda, Akashi chemical heat stove.Adopt self-propagating reaction system Ti+C as thermal source, the self-propagating reaction powder wrapped outside powder to be sintered, after the electric ignition mode is ignited,, by the self-sustaining reaction heat release, is treated sintered powder and carried out preheating.This method can prepare high purity tungsten and the tungsten-bast alloy of solid density more than 90%.The people's such as Chen Pengwan the patent (patent No.: 2007101632278) relate to a kind of self-spreading pre-heating powder aqueous medium bidirectional blasting and concreting device, for the preparation of the difficult fixed metal of high density (or pottery) composite and FGM thereof.This device adopts the form that is arranged symmetrically with, at two sample box intermediate arrangement self-propagating reaction powder that are arranged symmetrically with, after treating the sintering powder after refiring and being preheated to predetermined temperature, ignite high energy master explosive by the plane detonation of two two-way generations of detonating of the plane wave generator that is arranged symmetrically with, thereby and utilize aqueous medium to transmit the planar explosive shock wave and realize bidirectional blasting and concreting to powder, prepared relative density and reached 95.5% Mo/Cu FGM and relative density and reach 96.05% W (Mo)/Cu FGM.
The major advantage of synthetic (SHS) exothermic heat of reaction heating of self propagating high temperature is: thermal discharge is large, be swift in response and can realize In Situ Heating.Because the method does not need external heat source, by the in-situ chemical reaction heat release, powder is carried out preheating, therefore, the method is had relatively high expectations to the safety of explosive is heat insulation, simultaneously, due to needs placement of multiple layers heat-barrier material between explosive and powder, cause the shock motion situation complicated, be unfavorable for the accurate control of technological parameter.
Summary of the invention
In view of this, the invention provides a kind of split type high temperature preheating powder explosive sintering device, select chemical heat or electrical heating method to treat the preheating of sintering powder, sintering effect is good, can accurately control technological parameter.
Split type high temperature preheating powder explosive sintering device of the present invention comprises that shock wave charging assembly, controlled split assembly and high-temperature sample reclaim assembly, described shock wave charging assembly is used for generating explosion wave, and described high-temperature sample reclaims assembly and is used for carrying and preheating powder to be sintered; Described controlled split assembly is locked in described high-temperature sample with described shock wave charging assembly and reclaims the assembly top, so that described shock wave charging assembly and described high-temperature sample reclaim between assembly with air insulated, the described controlled split assembly described shock wave charging assembly of rear release that is triggered, contact so that described shock wave charging assembly reclaims assembly with described high-temperature sample.
Beneficial effect: split type high temperature preheating powder explosive sintering device provided by the invention utilizes controlled split assembly to realize locking and the release of shock wave charging assembly, need not explosive is carried out heat insulation processing, but by adjusting aqueous medium height, main explosive charge and explosive type fine adjustment blast impulse pressure and shock wave continuous action time, by selecting chemical heat method or electrical heating method, powder to be sintered is preheating to more than 1000 ℃, and can determines the Optimal Burst time according to sintering condition.
Description of drawings
Fig. 1 is split type high temperature preheating powder explosive sintering device pictorial diagram.
Fig. 2 is split type high temperature preheating powder explosive sintering apparatus structure schematic diagram.
Fig. 3 is controlled split mechanism action schematic diagram.
Fig. 4 is explosive sintering sample pictorial diagram.
Wherein, 1-electric cap, 2-guide rail, 3-booster gains, the 4-contiguous block, 5-explosive, the holder of 6-steel, 7-magnetic valve, the 8-spring, the 9-connecting rod, 10-retrains end cap, 11-long handle, 12-lateral momentum piece, 13-indicator light switch, 14-powder to be sintered, the 15-sample box, 16-heating unit, 17-sample box cushion block, the 18-heating container, 19-bottom momentum piece, 20-fixed platform.
The specific embodiment
, below in conjunction with the accompanying drawing embodiment that develops simultaneously, describe the present invention.
the invention provides a kind of split type high temperature preheating powder explosive sintering device, comprise the shock wave charging assembly, controlled split assembly and high-temperature sample reclaim assembly, Fig. 1 is device pictorial diagram of the present invention, the shock wave charging assembly of top is used for generating explosion wave, the high-temperature sample of below reclaims assembly and is used for carrying and preheating powder to be sintered, the shock wave charging assembly being locked in high-temperature sample at the controlled split assembly of side reclaims above assembly, make shock wave charging assembly and high-temperature sample reclaim between assembly with air insulated, but release of shock wave charging assembly after controlled split assembly is triggered, making shock wave charging assembly and high-temperature sample reclaim assembly contacts.
Fig. 2 is the structural representation of this device, and the shock wave charging assembly produces shock wave by explosive 5 blasts.High-temperature sample reclaims in assembly and is contained with and is preheating to both powders to be sintered of fixed temperature.Controlled split assembly comprises steel holder 6, guide rail 2, contiguous block 4, magnetic valve 7, long handle 11, connecting rod 9 and fixed platform 20.There is outstanding outer steel holder 6 both sides, and outer is slidably mounted on guide rail 2 by contiguous block 4, make steel holder 6 to move up and down; Magnetic valve 7 is fixed on fixed platform 20, and fixed platform 20 is fixed on guide rail, after the power connection of magnetic valve 7,11 moments of long handle is moved upward (as shown in Figure 3); Connecting rod 9 is fold-type (as Fig. 3 embodiment, being " ㄣ " type), and one end and long handle 11 lower ends are hinged, and middle part is fixed on fixed platform 20 with rotating shaft, and the other end is free end.While needing locking, free end is held the outer of steel holder 6 in the mode of taking of stumbling, and steel holder 6 is by locking; While need discharging, connect the power supply of magnetic valve 7,11 moments of long handle move upward, and drivening rod 9 rotates, and makes free end break away from the outer of steel holder, and the steel holder is released whereabouts.Wherein, magnetic valve 7 is selected from commercial, by circuit, is controlled; Guide rail 2 is the steel guide rail of diameter 6mm.
In certain embodiment, the shock wave charging assembly comprises the explosive unit, the explosive unit comprises electric cap 1, booster gains 3, explosive box and explosive 5, and the quality of the type of explosive 5 (as nitromethane, TNT, 8701 explosives, B explosive etc.) and explosive (is chosen according to concrete experiment condition as 0~500g).
In certain embodiment, the steel holder 6 in controlled split assembly has a groove, and in groove, for transmitting the medium of explosion wave, as aqueous medium, supporting lucite capping is sealed in the slot opening place, and medium and explosive are separated.
In certain embodiment, high-temperature sample reclaims assembly and comprises bottom momentum piece 19, lateral momentum piece 12, adds sample box 15 and hot cell 16.Bottom momentum piece 19 and lateral momentum piece 12 are steel, are used for eliminating the rarefaction wave that shock reflection forms, and wherein lateral momentum piece 12 is the hollow structure of upper and lower opening, and bottom is with 19 sealings of bottom momentum piece, and upper opening is to place heating unit 16; Sample box 15 is placed on heating unit 16 middle parts; Powder 14 to be sintered is suppressed in sample box 15 by press, is formed with the powder base of certain initial density; Heating unit 16 is taked chemical heat and two kinds of methods of electrical heating to treat sintered powder to carry out preheating as required.Sample box 15 is processed by 304 stainless steels, external diameter 30mm, and internal diameter 22mm, and can place on demand sample box cushion block 17.In addition, also can, at heating unit 16 top configuration constraint end caps 10, be steel at heating unit 16 exterior arrangement heating containers 18, to improve the explosive sintering effect.
During installation, shock wave charging assembly, controlled split assembly and high-temperature sample are reclaimed assembly install respectively, then guide rail 2 is welded on high-temperature sample recovery assembly, as Fig. 2 embodiment, be welded on lateral momentum piece 12; At this moment, (apart from high-temperature sample, reclaim assembly approximately 5~60mm) along guide rail 2 Mobile steel holders 6 to appropriate location, again the free end of connecting rod 9 is held the outer of steel holder 6 in the mode of taking of stumbling, thereby steel holder 6 is locked at current location, then the shock wave charging assembly is fixed in the steel holder; Reclaim assembly for high-temperature sample, powder 14 to be sintered is placed in sample box 15, sample box 15 outsides are heating unit 16, heating container 18, lateral momentum piece 12 and bottom momentum piece 19.Can be good to guarantee contact at contact site coating butter or vaseline during installation.
During use, treat sintering powder 14 with heating unit 16 and carry out preheating, after both reaching fixed temperature, connect the power supply of magnetic valve 7, long handle 11 moves upward, and drivening rod 9 rotates (Fig. 3 embodiment is for rotating counterclockwise), and the free end of connecting rod 9 breaks away from the outer of steel holder 6, steel holder 6 discharges whereabouts together with the shock wave charging assembly, falls at high-temperature sample and reclaims on assembly.This moment ignition charge 5, the explosion wave of formation to powder 14 to be sintered, carries out explosive sintering to it through steel holder, medium and 10 pressure transmissions of constraint end cap.
Further, at guide rail 2 lower end pocketed springs 8, use the spring of varying strength according to the quality sorting of shock wave charging assembly, when falling, plays the shock wave charging assembly on the one hand cushioning effect, while guaranteeing that lower backwardness clashes, explosive 5 can not spill or topple, guarantee on the other hand after the shock wave charging assembly is stable, steel holder 6 and constraint end cap 10 contact.
Further, indicator light switch 13 is installed on lateral momentum piece 12, can trigger indicator light switch 13 when the shock wave charging assembly falls to clashing into after high-temperature sample reclaims assembly, indicator light switch 13 connects outside indicator lamp, and when indicator lamp lights, prompting this moment can ignition charge 5.
Utilize device of the present invention can be prepared as follows process:
Experiment 1, the experiment of W90-Cu10 mixed-powder self-spreading pre-heating typical temperature increase
Utilize the chemical heat method, adopt (TiO 2+ Al+C)~(Fe 2O 3+ Al) certainly to spread mixed system be heating unit, wherein (Fe 2O 3+ Al) system is sneaked in 20%, 30% and 40% ratio.Adopt 2 12 volts (DGA-120) storage batterys to be composed in series the heavy current source, electric ignition tungsten filament two ends are connected with BLV and then with current source, are connected by electrical wire clip.Temperature rising history with diameter of phi 1mm K type thermocouple measurement powder center and peripheral place.Result shows, experience is approximately after 120s, and powder reaches maximum temperature, and reach Isothermal Condition, after this temperature starts slow decreasing, therefore, the Optimal Burst time should be elected 120s as, and the preheating maximum temperature can be regulated according to powder amount used, and whole device is reliable operation at high temperature.
Experiment 2, the experiment of W90-Cu10 mixed-powder self-spreading pre-heating explosive sintering
This experiment W powder used purity is greater than 99.9%, average grain diameter is 2 μ m, Cu powder purity is greater than 99%, and average grain diameter is 2 μ m, and the W powder mixes according to the mass ratio ratio of 9: 1 with the Cu powder, after the high-energy ball milling of 2 hours, the initial powder that obtains mixing, then suppress initial powder in sample box with hydraulic press, forms heavy wall tubulose machine and press from spreading powder, thickness is 16mm, and relative density is 60%.Adopt nitromethane liquid explosives (nitromethane: density 1.18g/cm3, detonation pressure 11.89GPa, explosion velocity 6300m/s, dose 200g).Adopt the chemical heat method identical with experiment 1, first machine is pressed from spreading powder and put into heating container, to put into machine by the fire hole on the heating container wall for the tungsten filament of igniting presses from the preformed hole that spreads on powder, pour that a little is loose from spreading powder as detonator into, the powder preheat temperature is the highest 770 ℃.Result shows, machine is pressed from spreading powder after the pre-heating temperature elevation explosive sintering, and sintering quality is good, and densification degree is high,, without obvious crackle, has higher turning ability.
Device of the present invention also can adopt Electric heating to the powder preheating,, for example take the solenoid resistance wire as heating unit, implements electrical heating around sample box.
Figure 4 shows that the diameter that utilizes apparatus of the present invention to obtain
Figure BDA0000149881670000071
W90/Cu10 explosive sintering sample
Pictorial diagram, its densification degree is higher, and without obvious crackle, turning ability is good, has showed good sintering quality.
In sum, these are only preferred embodiment of the present invention, not be used for limiting protection scope of the present invention.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.

Claims (4)

1. split type high temperature preheating powder explosive sintering device, it is characterized in that, comprise: shock wave charging assembly, controlled split assembly and high-temperature sample reclaim assembly, described shock wave charging assembly is used for generating explosion wave, and described high-temperature sample reclaims assembly and is used for carrying and preheating powder to be sintered; Described controlled split assembly is locked in described high-temperature sample with described shock wave charging assembly and reclaims the assembly top, so that described shock wave charging assembly and described high-temperature sample reclaim between assembly with air insulated, the described controlled split assembly described shock wave charging assembly of rear release that is triggered, contact so that described shock wave charging assembly reclaims assembly with described high-temperature sample;
Described controlled split assembly comprises steel holder (6), guide rail (2), contiguous block (4), magnetic valve (7), connecting rod (9), long handle (11) and fixed platform (20); Two described guide rails (2) are parallel to each other and vertically are welded on described high-temperature sample and reclaim on assembly, and there is outstanding outer described steel holder (6) both sides, and described outer is slidably mounted on guide rail (2) by contiguous block (4); Described fixed platform (20) is fixed on guide rail, magnetic valve (7) is fixed on described fixed platform (20), and connecting rod (9) is fold-type, and one end and long handle (11) lower end is hinged, middle part is fixed on fixed platform (20) with rotating shaft, and the other end is free end; The described free end mode of taking of can stumbling is held described outer, with described steel holder (6) locking; Long handle (11) moment is moved upward, drive described connecting rod (9) and rotate, so that described free end breaks away from described outer; Described shock wave charging assembly is placed in described steel holder (6);
Described high-temperature sample reclaims assembly and comprises bottom momentum piece (19), lateral momentum piece (12), heating container (18), sample box (15), heating unit (16) and constraint end cap (10); Described lateral momentum piece (12) is cylindrical structure, its below seals with described bottom momentum piece (19), described heating container (18) has groove, be positioned at the hollow position of described lateral momentum piece (12), described heating unit (16) is arranged in described groove, described heating unit (16) is cylindrical structure, and described sample box (15) is positioned over the hollow position of described heating unit (16); Described constraint end cap (10) is covered in described heating container (18) top.
2. device as claimed in claim 1, is characterized in that, described steel holder (6) has groove, and be furnished with the lucite capping, and described lucite capping is sealed in described slot opening place, and the medium that can transmit explosion wave is arranged in described groove.
3. device as claimed in claim 1, is characterized in that, described controlled split assembly further comprises the spring (8) that is set in guide rail (2) bottom.
4. device as claimed in claim 1, is characterized in that, indicator light switch (13) is equipped with in described lateral momentum piece (12) upper surface, when described shock wave charging assembly falls to striking after described high-temperature sample reclaims assembly, triggers indicator light switch (13).
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CN103317131B (en) * 2013-06-18 2016-03-02 北京科技大学 A kind of carbon nano tube-doped modification tungsten and explosive consolidation preparation method thereof
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CN111730732A (en) * 2020-06-23 2020-10-02 姜家吉 Process for improving advanced ceramic sintering yield
CN114029602B (en) * 2021-11-27 2023-02-21 北京理工大学 In-situ rapid self-propagating heating refractory metal explosion welding device and process
CN115971487B (en) * 2023-03-21 2023-06-09 东北大学 Neodymium iron boron magnet explosion pressing forming die and forming method

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