CN1593872A - Functional ceramic low voltage discharge compression forming method - Google Patents

Functional ceramic low voltage discharge compression forming method Download PDF

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Publication number
CN1593872A
CN1593872A CN 200410013314 CN200410013314A CN1593872A CN 1593872 A CN1593872 A CN 1593872A CN 200410013314 CN200410013314 CN 200410013314 CN 200410013314 A CN200410013314 A CN 200410013314A CN 1593872 A CN1593872 A CN 1593872A
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discharge
voltage
density
compacting
powder
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CN1323820C (en
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黄尚宇
陈堰波
李友成
吴彦春
孟正华
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a kind of press shaping method with low voltage discharge of the function ceramic. First put function ceramic powder that has been confected well in polyethylene alcohol solution to get mucus. Grind and griddle the mucus with a 40-hole screen. Put certain amount in concave module of the low voltage electromagnetism pressing mechanism and discharge to press with voltage 700~900 for one or two times, demould then get the finished product. The invention discharges instantly by energy storage capacitance to form a strong impulse magnetic field so as to shape the blank fast. The blank is pressed well and has high consistency and fine and even particle.

Description

Function ceramics low-voltage discharge method for press forming
Technical field
The present invention relates to ceramic material base substrate compact technique.Be particularly related to function ceramics low-voltage discharge method for press forming.
Background technology
Powder metallurgy is the effective way of producing work materials under various high performance structures materials, special type function material and the maximum conditions.In recent years, it has become from single material Manufacturing Technology Development and has melted the emerging technology science that material preparation, processing and shaping are machined in one, is the field, forward position of current material science development.Researching and developing effective high density, high-performance ceramic goods powder forming technology, is to promote ceramic material exploitation and the key for preparing.
With thump load pressing powdered material is the effective ways that obtain the high-density powder goods.Nineteen fifty-two, triumphant that metal company of the U.S. is mixed TiC, TaC and is sealed in the metal bag with the Ni powder, place the big breech piece of 355mm bore, the shock wave that is produced in the bore implode with explosive is shaped the powder pressurized, develop the cermet jet blade, opened research prelude with high energy rate forming (High Energy Rate Forming) method pressed powder goods.After this, various countries scholar and engineers and technicians launch research to this one after another, and achievement in research is to improving superhard powder compaction density and producing the large-scale performing member that can't suppress with general forcing press and played important function.But because problem such as blast compacting (Explosive Compaction) exists that process repeatability is poor, automaticity is low and security is relatively poor has limited applying of this technology.
Electro-magnetic forming (Electromagnetic Forming) is another kind of high energy rate forming method, and it is by high-voltage energy storage capacitor the coil instantaneous discharge to be produced strong pulsed magnetic field, makes blank impact high-rate forming under the electromagnetic force effect.Aspect shaping energy and speed control, electro-magnetic forming is better than explosive forming, and it does not need transmission medium, and forming process can be finished under vacuum environment.1976, Clyens, Johnson and Al-Hassani take the lead in the correlation technique of electro-magnetic forming is introduced the dusty material compacting, with discharge pressing (EDC, Electrical Discharge Compaction) suppresses the more complicated product of bar, billot and shape, by the screening powder size, they also successfully produce bar and the billot with wedge angle.This method has not only effectively overcome the limitation of blast compacting, and the fuel factor of utilizing the blockage effect (' Pinch ' Effect) of electromagnetic field and electric current will be suppressed with sintering process and be combined together, but, only depend on the contraction of electromagnetic field still to be not enough to process uniform high-density powder goods because of the Kelvin effect of high frequency electric.For this reason, the researcher is constantly improved it.Darvizeh adopts the compacting of discharging again after axially applying precompression, obtained the solder bar of stellite; Alp compacting (the 20Kv that will discharge, 18 μ F) and dynamically suppressing (dynamic compaction) combines, adopt discharge impact compacting (Electroimpact Compaction), goods compacted density and uniformity have been improved, and when surge reaches maximum, discharge, obtained the good pulverulent product of mechanical performance.To the nineties in 20th century, the discharge pressure sintering (PDPS or PAS, Pulse Discharge PressureSintering or Plasma Activated Sintering) that will suppress and the sintering process that grows up on this basis integrates begins widely, and people pay close attention to.Successful in this way realization the shaping processing of multiple superhard material, refractory alloy, function ceramics and function-graded material, goods have good crystalline phase tissue, residual stress is minimum, and is non-microcracked, wearability and impact resistance are fine.Weak point is that equipment cost is higher, makes complexity, has both needed the mechanical-force-transmission system, produces the device of pulse current again, and is also bigger to the mold materials loss.
Low-voltage discharge press forming (Low Voltage discharge Forming) is that the voltage of conventional high-tension electro-magnetic forming is reduced to hundreds of volts from thousands of volts to several ten thousand volts, guarantee the required discharge energy that is shaped by increasing electric capacity, like this, the equipment complexity reduces, volume greatly reduces, manufacturing cost significantly descends, and safety in utilization and reliability obviously improve, and the form-wound coil life-span also reduces effectively to prolong because of the discharge current amplitude.This technology starts from beginning of the nineties late 1980s, be mainly used in can not produce magnetic pad effect and loading speed should not too high occasion.At present, U.S. Electroimpact company has developed electromagnetic riveting (Electromagnetic Riveting) equipment of operating voltage below 1200V, obtain production application in companies such as North, Beoing, Alcoa, Lockheed, Textron, Douglas, LTV, British Aerospace, Chester, Avionsmarcel, occurred the problem of micro-crack when successfully having solved the aluminium alloy riveted joint because of loading speed is too fast.NORTHWEST CHINA polytechnical university begins to carry out the research work of Low Voltage Electromagnetic Riveting in the mid-90, discharge voltage is reduced to below the 450V; Wuhan University of Technology has developed the following electro-magnetic forming equipment of operating voltage 800V, and takes the lead in using it for the dusty material press forming, has obtained relative density and has reached 99% pulverulent product.
Dusty material low-voltage discharge press forming is to melt electricity, mechanics, powder metallurgy and machinery and material science in the powder forming new method for processing of one.
The electronic sensor that at present a lot of high-tech products are badly in need of is a large amount of, make with ceramic material, and the performance of this electron-like sensor depends on the compacted density of base substrate to a great extent, how to improve the base substrate compacted density? it is present urgent problem.
The ceramic body drawing method mainly contains injection forming, isostatic compaction, mechanical-moulded at present.Mechanical-mouldedly be divided into again: roll forming, plastic pressure forming, injection mo(u)lding, rolling formation, hydraulic pressure or mechanical pressure moulding.Because the special process requirement of sensor class function ceramics, its base substrate only is suitable for adopting hydraulic pressure or mechanical pressure moulding, but hydraulic forming equipment costs an arm and a leg, and in mechanical-moulded, because power can deficiency cause compacted density to be difficult to promote.With high-duty thump load press ceramic blank is the effective ways of producing the high density ceramic goods and obtaining its property.Wherein, electro-magnetic forming (ElectromagneticForming) is by high-voltage energy storage capacitor the coil instantaneous discharge to be produced strong pulsed magnetic field, makes blank impact high-rate forming under the electromagnetic force effect.Aspect shaping energy and speed control, electro-magnetic forming more is better than hydroforming, mechanical molding, is easy to obtain highdensity base substrate when the press ceramic powder.Be suitable for making, development of new electronic sensor features pottery,
Summary of the invention
The purpose of this invention is to provide a kind of function ceramics low-voltage discharge method for press forming.
Its low-voltage discharge method for press forming step is as follows:
(1) ceramic powder is levigate, add that to contain that polyvinyl alcohol 3wt%~the 5wt% aqueous solution is made binding agent wetting, ground 40 mesh sieves then;
(2) with the resulting powder of step (1), take by weighing set amount, put into low-voltage electromagnetism press device (storage capacitor 14350 μ F) die discharge compacting, discharge voltage 700~900V, discharge time 1~2 time;
(3) demoulding promptly gets the sample that is shaped, for sintering.
Adopt low-voltage discharge compression moulding technology.The ceramic powders that mixes is put into low-voltage electromagnetism press device mould, promote drift by driving chip, with high speed electromagnetic energy is changed into kinetic energy, act on the powder, make that powder particle moves, brittle fracture etc., thereby the filling space improves density, to reach the compacting purpose.
Description of drawings
Fig. 1 low-voltage electromagnetism pressing process equipment schematic diagram.
Fig. 2 blank relative density is pressed relation curve with discharge piezoelectricity.
Fig. 3 TiO 2The density of goods and the relation curve of suppressing voltage behind the sintering.
Fig. 4 TiO 2The goods stereoscan photograph that ceramic powder is suppressed with compacting of 900V electromagnetism and 200MPa tradition static pressure.
Number in the figure implication: 1 coil holder, 2 coils, 3 driving chips, 4 amplifiers, 5 drifts, 6 dies, 7 cover dies, 8 powders, 9 bases, 10 pull bars, 11 guide rods, 12 upper cover plates, 13 nuts.
Low-voltage electromagnetism press device shown in Figure 1, adopt indirect processing mode, actuating coil 2 is fixed together with coil holder 1, when discharge switch is closed, coil midstream is crossed a pulse current, driving amplifier 4 and drift 5 move downward red copper driving chip 3 together under the electromagnetic force effect impacting, and realize powder compaction.Driving chip and drift all are embedded in the amplifier, and the amplifier front end makes certain taper, are beneficial to the transmission and the amplification of stress wave.Guide rod 11 play the guiding role.Die 6 is done into two, with 7 one-tenth certain taperings of cover die, is convenient to take out pulverulent product.Drift and die material are No. 45 steel, not heat treatment.
The specific embodiment
Embodiment 1 uses TiO 2Powder is tested
One, experimentation:
1, is equipped with powder
With TiO 2Powder is earlier 1150 ° of pre-burnings, and insulation 4h makes it be converted into the rutile phase, places ball grinder to add absolute ethyl alcohol wet-milling 4h at high speed ball mill then, oven dry, and the hand mill, standby.
2, pressing process
During compacting at TiO 2Add the 4wt% poly-vinyl alcohol solution in the powder and make binding agent, addition is 2% of a powder weight, fully grinds in mortar then, crosses 40 mesh sieves.In the experiment of pressing, at first fix the quality of each pressed powder, change the discharge voltage parameter, between 400-1100v, suppress 10-15 sample every 100v.Secondly, change the quality of pressed powder, equally change voltage compacting sample, to analyze the influence of shape factor (ratio of height to diameter) to extrudate density by the front.In addition, adopt the compacting of not demoulding multiple discharge, to analyze the influence of repeatedly suppressing extrudate density.
3, sintering
Place crucible to put into high temperature furnace in goods, be warming up to 600 ℃, insulation 4h, discharge opeing glue.
Be placed on then and put into high temperature furnace heat-agglomerating in the corundum crucible.Sintering temperature is 1400 ℃, insulation 4h, 7 ℃/minute of the gradients of heating.In burner hearth with after the stove cooling, with its taking-up.
4, density measurement
The method of testing of green density is: measure the blank height, and diameter, quality is tried to achieve green density through calculating.The bulk density of goods adopts Archimedes's method (being drainage) test behind the sintering.The density measurement result of every group of sample discards the bigger several values of error, gets 10 sample density mean values at last.The powder solid density is 4.25g/cm 3
Two, density measurement result
The blank averag density distribution curve of test is seen Fig. 2, and the density profile of goods is seen Fig. 3 behind the sintering.
By Fig. 2,3 as can be seen, the density of compacting sample ascendant trend occurred before this with the increase of voltage under different powder qualities, when voltage increases reaches certain value, all began to occur descending, and showed as rapid decline in Fig. 3.Density all rises in gradient with the increase of voltage in suitable compacting voltage range, and under the lower condition of voltage, ascensional range is bigger, when voltage is higher, it is slow that ascensional range becomes gradually, even the situation that density no longer increases appears, and one section platform appears on density profile, show that this section voltage range is best compacting scope.With the powder quality is that 2g compacting sample is an example, and as can be seen from Figure 2, its blank amplification between the 500-700v discharge voltage is obvious, eases up at 700-900v, and the density downward trend occurs more than 900v.Therefore can think that 800-900v is for suppressing scope preferably with this understanding, after surpassing this scope, compacting situation instability may make ceramic inside layering occur, causes green density to descend on the contrary.This phenomenon Fig. 3 more significantly shows, and sharply descending appears in the blank of suppressing under 1000v density behind sintering, and this is because goods inner result who serious layering occurs behind sintering.Powder quality is that the sample of 2.5g and 3g also has similar result.The numerical value that shows discharge voltage in the electromagnetism compacting has higher influence for compact density, and certain discharge voltage is essential to moulding high density ceramic body, but simultaneously because the fragility voltage of pottery can not be too high.It is extremely important in technical process to choose suitable magnitude of voltage.
Under the equal in addition voltage, along with the increase of powder quality, density descends relatively.This mainly is owing to the increase along with powder quality, and the ratio of height to diameter of blank increases, the corresponding increase of the friction between powder and the die wall, and electromagnetic force expends and is overcoming the work increase of friction institute.Therefore all as can be seen, the discharge voltage the when blank that quality is bigger reaches maximum density value is also corresponding bigger by Fig. 2 Fig. 3.Powder of the same race is described, ratio of height to diameter difference, the optimum voltage scope of compacting are also different.
Can be clear that by Fig. 2 and Fig. 3 twice compacting improves obviously powder density, illustrate that twice compacting also is the effective way that obtains the high density blank.And for the homogenous quantities powder, the optimal discharge voltage when reaching high density is less than the optimal discharge voltage of the compacting of the single under the equal conditions.But twice compacting voltage can not be too high, when voltage increased to 900v, density no longer increased even occurs descending, and illustrates that base substrate inside has begun to occur defective, and goods serious layering occurs and break behind the sintering, therefore must the suitable discharge voltage of choosing twice compacting.
Three, comparative analysis
Same prescription is with traditional static pressure 200MPa compacting and the TiO that suppresses in the discharge of 700-900v discharge voltage condition 2Blank density sees Table 1,
The TiO of the different drawing methods of table 1 2The base substrate relative density
????TiO 2 ????m=2g ????m=2.5g ????m=3g
Green density g/cm 3 Static pressure The discharge compacting Static pressure The discharge compacting Static pressure The discharge compacting
??2.36 ???2.41~2.78 ??2.39 ???2.30~2.70 ???2.25 ???2.21~2.59
The maximum relative density % of blank ??55.5 ???65.4 ??53.8 ???63.5 ???52.9 ???60.9
Data declaration in the table 1, the ceramic blank density of suppressing under suitably high voltage all are higher than the green density of common static(al) compacting.This is because static(al) when compacting, powder elder generation compacting near drift, again press power is transmitted downwards, because the rubbing action of compacted powder and die wall, the press power that drift applies is when being delivered to the bottom, had greatly and offset, made extrudate density along the pressing direction distribution gradient by frictional force.The electromagnetism compacting is then different, inertia force plays a leading role in compacting process, pulse-electromagnetic force the upper strata powder as yet fully before the compacting promptly the form with stress wave pass to the powder bottom, the pressure transmission loss depends primarily on the wave resistance of dusty material, therefore, comparatively even along the pressing direction Density Distribution, thus make electromagnetism pressing blank density be higher than static pressure base volume density.
The TiO of different drawing methods 2The density of base substrate behind sintering sees Table 2
The TiO of the different drawing methods of table 2 2Goods relative density behind the blank sintering
????TiO 2 ????m=2g ????m=2.5g ????m=3g
Green density g/cm 3 Static pressure The discharge compacting Static pressure The discharge compacting Static pressure The discharge compacting
?3.91 ???3.9~3.96 ??3.87 ???3.85~3.92 ??3.84 ???3.78~3.85
The maximum relative density % of blank ?92 ???93.1 ??91.1 ???94 ??90.3 ???91
As can be seen from Table 2, compare the goods of sintering behind the static pressure, the extrudate density height that adopts the ceramic of suitable electromagnetism compacting parameter compacting to obtain behind same sintering process is as through twice compacting of 800v 2.5g TiO 2The goods relative density can reach 94%, has improved 3% than static pressure resulting product density, and this mainly is because the electromagnetism compacting has improved green density, has improved the sintering character of goods, makes extrudate density be improved.Therefore electromagnetism is suppressed the sintering character that increases ceramic blank density and improved ceramic body, finally improves extrudate density, and therefore can draw the electromagnetism compacting is a kind of effective forming method that obtains high fine and close function ceramics.
The TiO of different pressing mode compactings back sintering 2The sem photograph of goods as shown in Figure 4.As seen from Figure 4, obviously less through the goods crystallite dimension of electromagnetism compression moulding, pore-size is also less.Because sintering schedule is identical, the TiO of compacting under 900v 2Goods relative density (92.2%) therefore can draw with close through the relative density (92%) of static pressure resulting product, and the electromagnetism compacting can be played the effect that crystal grain thinning increases the crystal boundary contact area, helps improving the performance of ceramic.
Four, conclusion
When 1, the ceramic powders electromagnetism was suppressed, under certain magnitude of voltage, density increased in gradient with the voltage increase.Under the constant situation of other parameter conditions, there is the compacting voltage range an of the best.
2, with the increase of ratio of height to diameter, friction increases between powder and the die, and energy consumption increases, and sample density reduces.
3, twice compacting can increase ceramic body density.Depress in same electrical, twice compacting improves obviously density.During twice compacting, density also improves with voltage and increases.And the optimal discharge voltage of twice compacting is less than the optimal discharge voltage of single compacting.
What 4, low-voltage discharge was suppressed can play the effect that crystal grain thinning increases the crystal boundary contact area, helps improving the performance of ceramic.

Claims (1)

1, a kind of function ceramics method for press forming, its feature adopts the low-voltage discharge pressing, and its method step is as follows:
(1) ceramic powder is levigate, add that to contain that polyvinyl alcohol 3wt%~the 5wt% aqueous solution is made binding agent wetting, ground 40 mesh sieves then;
(2) with the resulting powder of step (1), take by weighing set amount, putting into storage capacitor is the low-voltage electromagnetism press device die discharge compacting of 14350 μ F, discharge voltage 700~900V, discharge time 1~2 time;
(3) demoulding promptly gets the sample that is shaped.
CNB2004100133141A 2004-06-18 2004-06-18 Functional ceramic low voltage discharge compression forming method Expired - Fee Related CN1323820C (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
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CN102248162A (en) * 2011-06-24 2011-11-23 宁波大学 Electromagnetically driven powder compacting device
CN103846431A (en) * 2012-11-28 2014-06-11 财团法人金属工业研究发展中心 Electromagnetic transmission compaction device and magnet manufacturing method
CN104625050A (en) * 2014-12-10 2015-05-20 武汉理工大学 Electromagnetic pressing manufacturing method for environment-friendly brazing filler metal foil
CN103846431B (en) * 2012-11-28 2016-11-30 财团法人金属工业研究发展中心 Electromagnetic driven compaction apparatus and Magnetitum manufacture method
CN108057883A (en) * 2018-01-02 2018-05-22 中南大学 The method and apparatus that a kind of radial and axial electromagnetic force realizes powder compacting
CN108172389A (en) * 2017-12-22 2018-06-15 哈尔滨工业大学 A kind of riveting assembling device and method of laminated structure part
CN109435308A (en) * 2018-12-19 2019-03-08 东莞市新日宝成形机器设备有限公司 A kind of powder compaction press
CN109663837A (en) * 2019-01-21 2019-04-23 福州大学 A kind of T-type profile corrector and its school type method
CN109986076A (en) * 2019-04-04 2019-07-09 武汉工程大学 A kind of ceramic particle enhancing electromagnetism hot pressed powder forming device and method

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CN1046172C (en) * 1996-12-31 1999-11-03 中国科学院等离子体物理研究所 Zinc oxide ceramic linear resistor and its producing method
CH693846A5 (en) * 1998-03-11 2004-03-15 Mitsubishi Electric Corp Compact electrode for discharge surface treatment
CN1247175A (en) * 1998-09-10 2000-03-15 上海赛科电子材料工程研究所 Dry pressing technology for integrally forming Si-Mo rod

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102248162A (en) * 2011-06-24 2011-11-23 宁波大学 Electromagnetically driven powder compacting device
CN103846431A (en) * 2012-11-28 2014-06-11 财团法人金属工业研究发展中心 Electromagnetic transmission compaction device and magnet manufacturing method
CN103846431B (en) * 2012-11-28 2016-11-30 财团法人金属工业研究发展中心 Electromagnetic driven compaction apparatus and Magnetitum manufacture method
CN104625050A (en) * 2014-12-10 2015-05-20 武汉理工大学 Electromagnetic pressing manufacturing method for environment-friendly brazing filler metal foil
CN108172389A (en) * 2017-12-22 2018-06-15 哈尔滨工业大学 A kind of riveting assembling device and method of laminated structure part
CN108057883A (en) * 2018-01-02 2018-05-22 中南大学 The method and apparatus that a kind of radial and axial electromagnetic force realizes powder compacting
CN109435308A (en) * 2018-12-19 2019-03-08 东莞市新日宝成形机器设备有限公司 A kind of powder compaction press
CN109663837A (en) * 2019-01-21 2019-04-23 福州大学 A kind of T-type profile corrector and its school type method
CN109986076A (en) * 2019-04-04 2019-07-09 武汉工程大学 A kind of ceramic particle enhancing electromagnetism hot pressed powder forming device and method

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