CN107716925B - A kind of super-pressure anti-slip mold for discharge plasma sintering - Google Patents

A kind of super-pressure anti-slip mold for discharge plasma sintering Download PDF

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Publication number
CN107716925B
CN107716925B CN201710888300.1A CN201710888300A CN107716925B CN 107716925 B CN107716925 B CN 107716925B CN 201710888300 A CN201710888300 A CN 201710888300A CN 107716925 B CN107716925 B CN 107716925B
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China
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ram
mold
cushion block
sintering
inner ram
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CN107716925A (en
Inventor
陈豫增
单贵斌
宫明明
董浩
张文祥
刘峰
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Northwestern Polytechnical University
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Northwestern Polytechnical University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10Sintering only
    • B22F3/105Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02Compacting only
    • B22F3/03Press-moulding apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2202/00Treatment under specific physical conditions
    • B22F2202/13Use of plasma

Abstract

The invention discloses a kind of super-pressure anti-slip mold for discharge plasma sintering, the components that the components shaped by high purity graphite and high-strength diamondite shape are composed;Wherein inner membrance is embedded in external mold inner sidewall boss top, and outer mold walls are equipped with radial blind holes, for installing thermocouple real-time monitoring temperature.The cavity that upper inner ram and lower inner ram are respectively embedded in the upper and lower part of internal model inner sidewall, and are formed between internal model is sintering zone, for loading the powder of sintering test specimen.Lower cushion block and upper cushion block one end are plane respectively against lower outer ram and upper outer ram, and other end is equipped with discoid protrusion, and are symmetrically installed respectively with lower inner ram, the cooperation of upper inner ram.Mold effectively improves the sintering pressure acted on sample under the premise of guaranteeing smoothly conductive, and can prevent interior external mold after mold long-time use from opposite slide occurring during the sintering process;To reduce production cost, production efficiency is improved.

Description

A kind of super-pressure anti-slip mold for discharge plasma sintering
Technical field
The present invention relates to powder metallurgy sintered equipment technical fields, specifically, being related to a kind of for plasma discharging burning The super-pressure anti-slip mold of knot.
Background technique
In recent years, nanocrystalline material because its excellent performance at home and abroad caused research upsurge, however due to preparation Technology is limited, is difficult to prepare large-scale bulk nanometer material at present.Opposite, nanometer crystal powder is prepared by high energy ball mill method The technology comparative maturity at end, therefore powder is prepared by lumpy nanometer crystalline substance material using powder metallurgy process and is had become currently The hot spot of research.Currently, mainly passing through hot isostatic pressing (HIP), ultra-high pressure sintering (UPS) and discharge plasma sintering (SPS) Method prepares bulk nanometer material.
Discharge plasma sintering method is that the powder such as metal are packed into mold made of the materials such as graphite, utilizes upper mold Pulse current and sintering pressure are applied to sintering powder by punching, bottom punch and powered electrode, through discharge activation, thermoplastic deformation and cold But a kind of novel powder metallurgy sintering technology of high performance material is produced.It is mainly characterized in that pulse direct current directly passes through graphite Mold is able to achieve the reachable 200K/min heating rate being exceedingly fast, with conventional sintering technique phase to generate a large amount of Joule heat Than that can realize the density close to theoretical value in the time under relatively low sintering temperature, shorter.But plasma discharging Sintering must be aided with special matched mold.
A kind of discharge plasma sintering mold is disclosed in patent of invention CN205200542U, which includes mold base With the mold set and seaming chuck that are located on mold base, the space that the inner wall of mold set surrounds forms mold cavity, and seaming chuck is from mould Has the upper end press-in die chamber of set;The lower section of the seaming chuck is equipped with upper tabletting, and the mold base is equipped with lower sheeting, upper pressure Piece and lower sheeting are slidingly sealed cooperation with the mold cavity respectively, in the space in mold cavity between upper tabletting and lower sheeting For the sintering zone of raw material powder.The mold can effectively avoid in vacuum-sintering the damage that instrument is caused because of the evolution of powder It is bad, discharge plasma sintering process preparation cost is reduced, while Mould operation is simple and convenient, improves production efficiency.However, by All it is integrally to be prepared by graphite, and the maximum pressure that conventional graphite is born is 50MPa or so in the mold, greatly limits Agglomerating plant maximum load, so that sintered specimen consistency is not high.
A kind of discharge plasma sintering mold is disclosed in patent CN202571280U, which successively covers including inside and outside Pressure head, mold set and the outer die casing connect, the space that the inner wall of mold set surrounds form mold cavity.Although the mold can be in certain journey Pressure when sintering is improved on degree, but since pressure head is still to be manufactured by graphite, the pressure that can be improved is limited.And if long Time uses, and the inside and outside die clearance of the mold can be gradually increased, and during the sintering process, interior external mold may occur to slide relatively, To cause the problem of falling of sample, the service life of mold is significantly reduced, the preparation cost of sample is increased.
Summary of the invention
In order to avoid the shortcomings of the prior art, the present invention proposes that a kind of super-pressure for discharge plasma sintering is anti- Slide mold;Shape zero of the components and high-strength diamondite that the mold is shaped by high purity graphite material Part combination effectively improves the sintering pressure acted on sample, greatly mentions under the premise of guaranteeing that mold can be smoothly conductive The consistency of high sintered type sample reduces sintering temperature, and passes through the design of external mold inner wall convex platform, prevents mold from making for a long time The problem of sliding opposite with rear generation, to reduce production cost, improve production efficiency.
The technical solution adopted by the present invention to solve the technical problems is: including external mold, internal model, lower outer ram, upper external pressure Head, lower inner ram, upper inner ram, lower cushion block, upper cushion block, the external mold are the hollow cavity of upper and lower ends opening, external mold inside Circumferentially arranged with boss on wall, inner membrance, which is embedded in external mold, is located at side wall boss top, and outer mold walls are equipped with radial blind holes, are used for Thermocouple real-time monitoring temperature is installed;The upper inner ram and the lower inner ram are the identical roundlet cylindrical portion of two structures Part, both ends are plane, and upper inner ram and lower inner ram are respectively embedded in internal model inner sidewall upper portion and lower part, and upper inner ram is under The cavity formed between inner ram and internal model is sintering zone, for loading the powder of sintering test specimen;Upper cushion block and upper outer ram according to The secondary top for being placed on inner ram, lower cushion block and lower outer ram are placed sequentially in the lower part of lower inner ram;The lower cushion block with The upper cushion block is the identical component of two structures, and lower cushion block and upper cushion block one end are plane respectively against lower outer ram and upper outer The other end of pressure head, lower cushion block and upper cushion block is equipped with discoid protrusion, and symmetrical with lower inner ram, the cooperation of upper inner ram respectively Installation.
External mold, internal model, lower outer ram and upper outer ram are all made of high purity graphite material.
Lower inner ram, upper inner ram, lower cushion block and upper cushion block are all made of high-strength tungsten carbide alloy material.
In the inner wall of internal model, the lower inner ram end face opposite with upper inner ram sprays boron nitride.
Beneficial effect
A kind of super-pressure anti-slip mold for discharge plasma sintering proposed by the present invention, is added by high purity graphite material The components that the components and high-strength tungsten carbide alloy material of work forming shape are composed;It is provided on mold for heat The thermometer hole of galvanic couple thermometric.Under the premise of guaranteeing that mold is smoothly conductive, the sintering pressure acted on sample is effectively improved, The consistency of sintered specimen is improved, sintering temperature is reduced.And it by the design of mold, is effectively prevented mold and uses for a long time Opposite the problem of sliding, occurs during the sintering process for interior external mold afterwards, to reduce production cost, improves production efficiency.
A. traditional discharge plasma sintering mold is made of graphite, and the limiting pressure that graphite material can bear is 50Mpa.By the design of mold, in the case where not influencing conductive capability, the Upper gasket of mold, lower gasket, upper inner ram, under Inner ram is shaped by high-strength tungsten carbide alloy material, and the pressure that high-purity tungsten carbide alloy material can be born reaches 1Gpa, because And nearly 20 times of boost in pressure are born, the consistency of sintered specimen is greatly promoted, and reduce sintering temperature, to improve production Efficiency reduces production cost.
B. after prolonged use, the gap between external mold and internal model can become larger conventional discharge plasma agglomeration mold, lead The two can occur to slide relatively during the sintering process for cause, so that sintering cannot continue.On the external mold inner wall of mold Boss structure is devised, is aided with the reasonable cooperation of size, is effectively prevented falling off for inside and outside mould, when shortening the dress of sample and taking Between, reduce the damage to mold.
Detailed description of the invention
With reference to the accompanying drawing with embodiment to a kind of anti-skidding stamping die of super-pressure for discharge plasma sintering of the invention Tool is described in further detail.
Fig. 1 is the super-pressure anti-slip mold structure diagram for discharge plasma sintering.
Fig. 2 is the super-pressure anti-slip die cut view for discharge plasma sintering.
In figure
1. on the lower inner ram 4. of 2. inner membrance 3. of external mold on 5. lower cushion block 6. of inner ram on the lower outer ram 8. of cushion block 7. Outer ram
Specific embodiment
The present embodiment is a kind of super-pressure anti-slip mold for discharge plasma sintering;First received what is prepared in advance Rice crystalline flour end is placed in the sintering zone formed by internal model, upper inner ram and lower inner ram, it is ensured that powder is close in sintering zone Filling.When work, mold is placed in discharging plasma sintering equipment, is powered so that the heating of entire mold thermally equivalent, with Pressure acts on outer ram simultaneously for this.It pushes cushion block mobile to mould inside, by ladder power transmission, finally pressure is applied to On powdered sample, so that powdered sample is sintered under pressure.The pressure that can be provided due to discharging plasma sintering equipment Power is limited, but can effectively improve burning so that the pressure acted on sample greatly increases by high-strength tungsten carbide ladder power transmission The consistency of sample is tied, and improves production efficiency, reduces production cost.
Refering to fig. 1, Fig. 2, it is anti-to the super-pressure for discharge plasma sintering below with reference to the sintering process of nano crystal iron Mold is slid to be described further.
In the present embodiment, for the super-pressure anti-slip mold of discharge plasma sintering, by external mold 1, internal model 2, lower external pressure First 7, upper outer ram 8, lower inner ram 3, upper inner ram 4, lower cushion block 5, upper cushion block 6 form;Wherein, external mold 1 is opened for upper and lower ends Mouthful cylindrical hollow cavity, circumferentially arranged with boss on 1 inner sidewall of external mold, inner membrance 2, which is embedded in external mold 1, is located at side wall boss Top, the boss design of external mold inner wall effectively prevent the opposite sliding of mold during the sintering process.Radial direction is provided on 1 wall of external mold Blind hole, for installing thermocouple real-time monitoring temperature.Upper inner ram 4 and lower inner ram 3 are the identical roundlet cylindricality of two structures Component, both ends are plane;Upper inner ram 4 and lower inner ram 3 are respectively embedded under 2 inner sidewall of 2 inner sidewall upper portion of internal model and internal model Portion, and the cavity formed between upper inner ram 4 and lower inner ram 3 and internal model 2 is sintering zone, for loading the powder of sintering test specimen End.Upper cushion block 6 and upper outer ram 8 are placed sequentially in the top of inner ram 4, and lower cushion block 5 and lower outer ram 7 are placed sequentially in down The lower part of inner ram 3.Lower cushion block 5 and upper cushion block 6 are the identical component of two structures, and lower cushion block 5 and upper 6 one end of cushion block are plane Respectively against lower outer ram 7 and upper outer ram 8, the other end of lower cushion block 5 and upper cushion block 6 is equipped with discoid protrusion, and respectively It is symmetrically installed with lower inner ram 3, the cooperation of upper inner ram 4.
In the present embodiment, external mold 1, internal model 2, lower outer ram 7 and upper outer ram 8 are all made of the processing of high purity graphite material.Under Inner ram 3, upper inner ram 4, lower cushion block 5 and upper cushion block 6 are all made of high-strength tungsten carbide alloy material processing.When mold assembles, The inner wall of internal model 2, lower inner ram 3 end face opposite with upper inner ram 4 spray boron nitride.
In the present embodiment, radial blind holes diameter is 1.1mm on 1 wall of external mold.In boss structure on 1 inner wall of external mold is capable of fixing The relative position of mould and external mold facilitates the dress of sample to take, and effectively prevent interior external mold after mold long-time use that opposite sliding occurs. It is powder sintered area by the cavity that internal model, lower inner ram and upper inner ram are formed;By formula P=F/S it is found that when equipment can be applied When the power added is certain, external mold 1 improves pressure by reducing sectional area.Therefore, the end face of lower cushion block 5 and upper cushion block 6 Equipped with discoid convex shape, ladder power transmission is formed, power is finally acted on the smaller lower inner ram 3 of cross-sectional area and upper internal pressure On first 4, plays a part of to increase pressure, realize ultra-high pressure sintering.
Experimentation:
It first checks whether mold has the case where cracking damage before being sintered dress sample, more renew mould immediately if any need Tool, in order to avoid occur unexpected, damage discharging plasma sintering equipment during the sintering process;
Before being packed into nanocrystalline iron powder, in the inner wall of internal model 2, the end face of lower inner ram 3 and upper inner ram 4 sprays nitridation Boron facilitates the sampling work after the completion of sintering;
After lower inner ram 3 is assembled with internal model 2, manocrystalline powders are packed into the cavity of the two formation, and by upper interior The powder pressure that pressure head 4 cooperates baby press to be loaded into is tight, it is ensured that the powder sintered of loading goes out to meet the style of requirement of experiment;
It after powder is packed into, by structure composable mold, and is put into discharging plasma sintering equipment, thermocouple is inserted in outer In the reserved blind hole of mould outer wall, the fire door of discharging plasma sintering equipment is shut, extracts vacuum, while writing control on computers Mild pressure control program, when vacuum degree is lower than 10-2When Pa, it is sintered experiment;
In sintering process, the voltage and current values that discharging plasma sintering equipment is shown are observed in real time, and pay attention to observing The working condition of mold, if cracking occurs for mold, situation should stop testing immediately;
After sintering, style furnace cooling is allowed to open fire door when temperature is lower than 150 DEG C, takes out sample, experiment knot Beam.

Claims (3)

1. a kind of super-pressure anti-slip mold for discharge plasma sintering, including external mold, internal model, lower outer ram, upper external pressure Head, lower inner ram, upper inner ram, lower cushion block, upper cushion block, it is characterised in that: the external mold is the hollow cavity of upper and lower ends opening Body, circumferentially arranged with boss on external mold inner sidewall, internal model, which is embedded in external mold, is located at side wall boss top, and outer mold walls are equipped with diameter To blind hole, for installing thermocouple real-time monitoring temperature;The upper inner ram is that two structures are identical with the lower inner ram Roundlet cylindrical part, both ends are plane, and upper inner ram and lower inner ram are respectively embedded in internal model inner sidewall upper portion and lower part, and on Inner ram and the lower cavity formed between inner ram and internal model are sintering zone, for loading the powder of sintering test specimen, in internal model Inner wall, the lower inner ram end face opposite with upper inner ram spray boron nitride;Upper cushion block and upper outer ram are placed sequentially in internal pressure The top of head, lower cushion block and lower outer ram are placed sequentially in the lower part of lower inner ram;The lower cushion block and the upper cushion block are two The identical component of a structure, lower cushion block and upper cushion block one end are plane respectively against lower outer ram and upper outer ram, lower cushion block with The other end of upper cushion block is equipped with discoid protrusion, and is symmetrically installed respectively with lower inner ram, the cooperation of upper inner ram.
2. the super-pressure anti-slip mold according to claim 1 for discharge plasma sintering, it is characterised in that: outer Mould, internal model, lower outer ram and upper outer ram are all made of high purity graphite material.
3. the super-pressure anti-slip mold according to claim 1 for discharge plasma sintering, it is characterised in that: in lower Pressure head, upper inner ram, lower cushion block and upper cushion block are all made of high-strength tungsten carbide alloy material.
CN201710888300.1A 2017-09-27 2017-09-27 A kind of super-pressure anti-slip mold for discharge plasma sintering Active CN107716925B (en)

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