CN104525943A - Pressurizing device for preparing high-density ultrafine grain tungsten block and application of pressurizing device - Google Patents
Pressurizing device for preparing high-density ultrafine grain tungsten block and application of pressurizing device Download PDFInfo
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Abstract
The invention relates to a pressurizing device for preparing a high-density ultrafine grain tungsten block and application of the pressurizing device. A pressing head is characterized in that the axial direction is the pressure applying direction; the pressing head is equipped with at least two sections in the axial direction; the section far away from a sample to be pressed is a remote end section which is prepared from graphite, and while the section in direct contact with the sample to be pressed is prepared from silicon carbide; the diameter of each section of the pressing head is sequentially increased in the direction far away from the sample to be pressed. The pressing head can be applied to the preparation of rare metals. According to the pressing head, the graphite section and the silicon carbide at different section are matched to achieve the purposes of applying pressure not greater than 100MPa to the graphite section and pressure exceeding 1GPa can be transmitted through the sample, and the problem of sintering at the high pressure can be solved.
Description
Technical field
The present invention relates to moulding shaping and PM technique, be specifically related to a kind of pressue device and the application thereof of preparing high fine and close superfine crystal tungsten block.
Background technology
Tungsten material is a kind of important rare metal, because it has high density, high-melting-point and excellent electron emission capability, is used in high-temperature work environment of being everlasting.Because at high temperature it still can keep good mechanical property, in aerospace field, nuclear power station, medical treatment detection device, tungsten material is obtained for and applies widely at present.The tungsten block of suitability for industrialized production generally adopts high temperature hydrogen furnace or vaccum sensitive stove sintering, this technique needs the temperature more than 2000 DEG C long-time (generally more than 10 hours) to sinter, but the density of the tungsten block sintered out can only reach about 90%, and because sintering temperature is high, sintering time is long, the tungsten block microscopic structure prepared is comparatively large, so just causes the mechanical property of material obviously to reduce.High-temperature hot isostatic sintering and high temperature hot pressing sintering technology sintered tungsten block can be used in addition, but these sintering technologies also need higher temperature and longer sintering time, the coarse microstructure of the tungsten block prepared, poor-performing, and also the cost of sintering is very high.
Now research direction has all focused on and how to have realized low temperature by increasing researcher, high pressure, Fast Sintering go out on high performance tungsten material.Patent 200410080350 " preparation method of low-temperature primary sintering high-density superfine crystal particle pure tungsten material " is exactly suppress growing up of material structure by reducing sintering temperature, prepare the pure tungsten material of ultra-fine grain, it is that pressed compact is shaping in a mold for the 70nm tungsten powder oneself prepared, then sinter molding in molybdenum wire furnace, the pure tungsten material density prepared is 95% ~ 96%, mean tungsten size of microcrystal Wei≤8 ~ 15 μm.Patent CN 100558923C " a kind of high specific gravity tungsten alloy material and preparation method for nano crystal block thereof thereof " is by adopting square wave direct current pulse-continuous current flash sintering method in addition, be prepare ultra-fine grain high specific gravity tungsten alloy material in 3 ~ 8 minutes by Stress control at 40MPa ~ 50MPa, sintering time, but density is lower.
Along with improvement and the development of sintering technology, vacuum discharge plasma sintering technology is adopted by increasing researcher.Because general sintering technology (normal pressure-sintered, hot pressing and sintering technique, HIP sintering technology) normally carries out more than the recrystallization temperature of material, it is a kind of process with diffusion, too high for sintering temperature material, time is also long, cause the coarse grains of the material prepared, mechanical property obviously reduces.Vacuum discharge plasma sintering technology (SPS sintering technology) is that the mode heated by DC pulse current is heated, this technology is the spark discharge phenomenon heating caused by pulse current, achieve material to heat from outside to inside, sintering time and temperature obviously reduce.University of Science & Technology, Beijing Zhang Pingping in 2012 etc. have studied " nanometer tantalum carbide is on the microstructural impact of SPS sintered tungsten ", they prepare by SPS sintering technology the tungsten briquet that average grain size is 22.19 μm, but because their sintering pressure is too low, the material density prepared is low.
Summary of the invention
For defect of the prior art and deficiency, the object of the present invention is to provide a kind of pressure head, pressue device and the application in rare metal preparation thereof, said apparatus is particularly utilized to prepare high fine and close superfine crystal tungsten block, solve and realize super-pressure, vacuum, low temperature and a short time sintering technology difficult problem in vacuum discharge plasma sintering furnace, the tungsten block even tissue making to prepare, near complete fine and close and crystal grain is tiny.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of pressure head, the axis of this pressure head is the direction of exerting pressure of pressure head, and described pressure head is axially arranged with at least two-stage along it, wherein away from treating that the one-level of pressure-like product is far-end level, the material of this far-end level is graphite, and treats that the material of the one-level that pressure-like product directly contact is carborundum.
Further, the diameter edge at different levels of described pressure head is away from treating that the direction of pressure-like product increases successively.
Further, on described pressure head, material is the level of graphite is graphite linings, and material is the level of carborundum is silicon carbide layer, and wherein: be provided with silicon carbide plate between adjacent graphite linings and silicon carbide layer, and the diameter of silicon carbide plate is identical with the diameter of graphite linings.
Additionally provide a kind of pressue device, this pressue device comprises described pressure head and graphite jig cover, and the far-end level of described pressure head is electrically connected between overlapping with graphite jig.
Further, described graphite jig cover comprises at least two-stage, is provided with the corresponding stage of pressure head in graphite jig cover at different levels.
Give the application of described pressure head for the preparation of rare metal simultaneously.
Give the application of described pressue device for the preparation of rare metal simultaneously.
Further give, described rare metal is tungsten.
Give, described application comprise particle diameter be 50 ~ 100nm tungsten powder pressure be 300MPa ~ 1GPa, temperature carries out sintering obtained tungsten block under be 1200 ~ 1500 DEG C and vacuum being the condition of 0.1Pa, the time wherein sintered is 3 ~ 15min.
Concrete, the density of described tungsten block is 93% ~ 99%, and the crystallite dimension of tungsten block is 0.6 ~ 1.5 μm, and the vickers microhardness of tungsten block is 520 ~ 680kg/mm
2.
The present invention compared with prior art, has the following advantages:
(1) pressure head of the present invention, by the graphite linings of different-diameter and coordinating of silicon carbide layer, achieve pressure graphite linings being no more than to 100MPa, sample can transmit the object of more than 1GPa pressure, ensure that the condition that also can realize giving sample high pressure while vacuum discharge plasma sintering furnace needs graphite to carry out conduction pulses current flow heats;
(2) the present invention is by the Process Exploration to concrete sintering temperature, pressure and sintering time, obtains the tungsten block of different density, crystal grain and hardness, meet different application requirements under the condition of different pressure, temperature and sintering time;
(3) the fine and close super Ultra-fine Grained pure tungsten block of the height prepared of the present invention, density reaches 93% ~ 99%, crystallite dimension reaches 0.6 ~ 1.5 μm and vickers microhardness reaches 520 ~ 680kg/mm
2, substantially improve the comprehensive mechanical property of tungsten block of material.
Accompanying drawing explanation
Fig. 1 is the sectional view of the pressue device described in the present invention;
Fig. 2 is the SEM organization chart of tungsten block prepared by embodiment three;
Fig. 3 is the SEM organization chart of tungsten block prepared by embodiment four;
Fig. 4 is the SEM organization chart of tungsten block prepared by embodiment five;
Fig. 5 is the SEM organization chart of tungsten block prepared by embodiment six;
Fig. 6 is the SEM organization chart of tungsten block prepared by embodiment seven;
Fig. 7 is the SEM organization chart of tungsten block prepared by embodiment eight;
Label in Fig. 1 is expressed as: 1 three grades of graphite jig covers, 1-1 secondary graphite jig cover, 1-2 one-level graphite jig cover, 101 thermometer holes, 2 tertiary carbon SiClx depression bars, 2-1 secondary carborundum depression bar, 2-2 one-level graphite depression bar, 201 silicon carbide plates, 3-sample;
Below in conjunction with specification drawings and specific embodiments, the present invention will be described.
Detailed description of the invention
Vacuum discharge plasma agglomeration is when DC-pulse is flowed through powder particle, produce discharge plasma instantaneously between particles, sintered body each uniform particles ground inner is made self to produce Joule heat and particle surface is activated, thus the block making powder sintered one-tenth fine and close.Therefore, it has sintering quick heating, and sintering time is short, and sintering temperature is low, the feature of homogeneous heating.Compared with traditional sintering, growing up of crystal grain can be suppressed, and reduce heat loss, improve sintering efficiency, the pulse current of discharge plasma sintering is transmitted by graphite linings and graphite jig cover, realize pulse current discharging sintering processing, but because the pressure-bearing of the graphite depression bar wherein conducted electricity can not more than 100MPa, limit the lifting of its pressure, pressure can not reach the pressure condition of more than the 1GPa in the present invention, therefore inventors performed the design of pressure head and pressue device, the maximum compressive resistance of SiC can reach 3 ~ 4GPa, the material of far-end level (level namely contacted with forcing press in vacuum discharge plasma agglomeration stove) is graphite, graphite pressure head from sample far-end is arranged on the Pressure Actuated Device of vacuum discharge plasma sintering furnace, distortion can not be produced under the graphite electric current transmission that namely can realize in sintering process also can bear the temperature of increasing simultaneously, guarantee is electrically heated needs under leading high temperature, with treat that the material of the one-level that pressure-like product directly contact is carborundum, the diameter at different levels of pressure head along away from treating that the direction of pressure-like product increases successively, realizing pressure increase at double and transmission, solving the problem that graphite depression bar can not bear high pressure,
Simultaneously, in order to reach different pressure demand, pressue device can be arranged to the combination that various level pressure head overlaps from the graphite jig of different progression, to reaching predetermined pressure requirements, it is one-level that pressue device in the present invention limits coordinating that a level layer of pressure head and a graphite jig overlap, and can carry out secondary, three grades even design of more than three grades pressue devices by different pressure requirements;
For three times' lifting device, three times' lifting device comprises three stage heads and three grades of graphite jig covers, secondary graphite jig cover and one-level graphite jig covers, and three stage heads comprise tertiary carbon SiClx layer, secondary silicon carbide layer and one-level graphite linings,
The fixing of sample is carried out in the periphery that the periphery that three grades of graphite jigs cover is closely linked in the periphery of tertiary carbon SiClx layer, secondary graphite jig cover is closely linked in secondary silicon carbide layer and one-level graphite jig cover are closely linked in one-level graphite linings, and one-level graphite linings is overlapped with one-level graphite jig cover, secondary graphite jig cover, three grades of graphite jigs and waits to press sample room to be electrically connected.
Far-end level and with treat the carborundum that multi-layer can be set in the middle of level that pressure-like product directly contact, and the diameter of each level of intergrade edge is away from treating that the direction of pressure-like product increases successively, the corresponding graphite jig coordinated with intermediate level overlaps and also arranges multilayer, to ensure the electrical connection of sample preparation.
In addition, in order to make the more tight of level interlayer compacting adjacent on pressure head, ensure that outermost graphite linings can not be crushed, between graphite linings and silicon carbide layer, place silicon carbide plate, the diameter of silicon carbide plate is identical with the diameter of graphite linings bottom surface.
The present invention is that the control of 0.1Pa condition is carried out sintering and prepared tungsten block by carrying out high pressure 300MPa ~ 1Gpa, high temperature 1200 ~ 1500 DEG C and vacuum to nano level tungsten powder, the density of the tungsten block obtained is 93% ~ 99%, the crystallite dimension of tungsten block is 0.6 ~ 1.5 μm, and the vickers microhardness of tungsten block is 520 ~ 680kg/mm
2, combination property is greatly improved; Further research shows, at the same pressure and temperature, the mechanical property of the tungsten block that different sintering times obtains also can be different;
The tungsten powder that the present invention prepares tungsten block can adopt ammonium metatungstate to be tungsten source, is prepared by sol-gal process and hydrogen reduction process, and the particle diameter of the tungsten powder of preparation is 50 ~ 100nm; Optional tungsten powder is prepared by following steps: step one: adopt ammonium metatungstate to be tungsten source, prepare WO by sol-gal process
3powder; Step 2: WO prepared by step one
3powder after 500 DEG C of reduction, then is 50 ~ 100nm tungsten powder at 800 DEG C of obtained particle diameters of reduction.
Tungsten block of the present invention, its density is 93% ~ 99%, and the crystallite dimension of tungsten block is 0.6 ~ 1.5 μm, and the vickers microhardness of tungsten block is 520 ~ 680kg/mm
2, compared with the tungsten block of the density 90% ~ 95% of existing tungsten block, crystallite dimension about 50 μm, in the present invention, the comprehensive mechanical property of tungsten block significantly improves.
Pressue device in the present invention can also be applicable in the preparation of the Rare Metals Materials such as molybdenum, titanium, zirconium.
Embodiment one: prepare tungsten powder
Step one: adopt ammonium metatungstate to be tungsten source, prepare nanometer WO by sol-gal process
3powder;
Step 2: by the nanometer WO of preparation
3powder reduces in plant hydrogen reduction furnace, in two steps: the first step was 500 DEG C of reduction 3 hours, and second step obtains 800 DEG C of reduction the nano-tungsten powder that particle diameter is 50 ran for 3 hours.
Embodiment two: pressue device
As shown in Figure 1: the pressue device described in the present embodiment is three times' lifting device, three times' lifting device comprises: three grades of graphite jig covers 1, secondary graphite jig cover 1-1, one-level graphite jigs overlap 1-2, tertiary carbon SiClx depression bar 2, secondary carborundum depression bar 2-1 and one-level graphite depression bar 2-2
Wherein three grades of graphite jig covers 1, secondary graphite jig cover 1-1 and one-level graphite jigs overlap the cylinder-like part that 1-2 is different inner diameters, three grades of graphite jig covers 1 are at interior depression bar, secondary graphite jig cover 1-1 and one-level graphite jig cover 1-2 and three grades of graphite jigs overlaps 1 coaxial fit successively, and the height that three grades of graphite jigs overlap 1 from inside to outside, secondary graphite jig overlaps 1-1 and one-level graphite jig overlaps 1-2 increases successively;
The sidewall of secondary graphite jig cover 1-1 and one-level graphite jig cover 1-2 is provided with thermometer hole 101, and the axis that thermometer hole 101 overlaps perpendicular to mould is arranged, and can place the thermometric components and parts such as thermocouple or monitor as the temperature of infrared temperature instrument hole to test specimen;
Tertiary carbon SiClx depression bar 2, secondary carborundum depression bar 2-1 and one-level graphite depression bar 2-2 successively arranged in co-axial alignment pressing carry out the transmission of pressure; Tertiary carbon SiClx depression bar 2 has two, and on two tertiary carbon SiClx depression bars 2 upper bottom surface of being axially oppositely arranged on cylindrical sample and bottom surface, three grades of graphite jigs covers 1 are closely linked in the periphery of two tertiary carbon SiClx depression bars 2; Same secondary graphite jig cover 1-1 is closely linked in the periphery of secondary carborundum depression bar 2-1, and one-level graphite jig cover 1-2 is closely linked in the periphery of one-level graphite depression bar 2-2;
In order to prevent adjacent secondary carborundum depression bar 2-1, one-level graphite depression bar 2-2 is crushed, and close contact between two depression bars can be ensured, ensure the pressure of forward, between secondary carborundum depression bar 2-1 and one-level graphite depression bar 2-2, place silicon carbide plate 201, the diameter of silicon carbide plate 201 is identical with the diameter of one-level graphite depression bar 2-2.
Make pressure increase in pressure transfer process by the change of the depression bar sectional area assembling different brackets, the pressure be finally delivered on powder can increase many times, and can realize being pressurized to multiple force value; The three times' lifting device of the present embodiment is arranged on the forcing press of vacuum discharge plasma sintering furnace, realizes the transmission of pressure.
Embodiment three: prepare tungsten block
(1) by calculating the pressue device of concrete size and grade:
By the tungsten block that the pre-prepared diameter of three times' lifting device in embodiment two is 10mm, one-level graphite depression bar 2-2 pressure is 90MPa, and the diameter of secondary carborundum depression bar 2-1 is 20mm, and preparing pressure needed for tungsten block is 1GPa;
Namely the diameter of tertiary carbon SiClx depression bar 2 is 10mm, and tertiary carbon SiClx depression bar 2 pressure is 1GPa, with P
1represent tertiary carbon SiClx depression bar 2 pressure, S
1represent the area of the pressure face of tertiary carbon SiClx depression bar 2, P
2represent secondary carborundum depression bar 2-1 pressure, S
2represent the area of the pressure face of secondary carborundum depression bar 2-1, P
3represent one-level graphite depression bar 2-2 pressure, S
3represent the area of the pressure face of one-level graphite depression bar 2-2;
Pass through formula: P
3s
3=P
2s
2=P
1s
1,
calculating secondary carborundum depression bar 2-1 pressure is 250MPa, then one-level graphite depression bar 2-2 diameter is 33.4mm; The internal diameter of three grades of graphite jig covers 1 is 10mm, and the internal diameter of secondary graphite jig cover 1-1 is 20mm, and the internal diameter of one-level graphite jig cover 1-2 is 33.4mm;
(2) tungsten block is prepared:
Tungsten powder embodiment one prepared loads in the three times' lifting device of size in (1), three times' lifting device is loaded in vacuum discharge plasma sintering furnace, control sintering temperature 1200 DEG C, vacuum is 0.1Pa, sintering time 5 minutes, forcing press is 90MPa to the pressure of one-level graphite depression bar 2-2;
As shown in Figure 2, obtaining tungsten block density is 98.1%, and average grain size is 878nm, and vickers microhardness is 563.11kg/mm
2.
Embodiment four: prepare tungsten block
With embodiment three unlike the sintering time in (2) 3 minutes;
As shown in Figure 3: the tungsten block density obtained is 95.4%, and average grain size is 859nm, and vickers microhardness is 550.52kg/mm
2.
Embodiment five: prepare tungsten block
(1) by calculating the pressue device of concrete size and grade:
Three times' lifting device in embodiment two is removed one-level graphite depression bar 2-2 and one-level graphite jig cover 1-2 obtain two-stage pressurizing device, by the tungsten block that the pre-prepared diameter of two-stage pressurizing device is 10mm, secondary carborundum depression bar 2-1 pressure is 90MPa, and preparing pressure needed for tungsten block is 600MPa;
Namely the diameter of tertiary carbon SiClx depression bar 2 is 10mm, and tertiary carbon SiClx depression bar 2 pressure is 600MPa, with P
1represent tertiary carbon SiClx depression bar 2 pressure, S
1represent the area of the pressure face of tertiary carbon SiClx depression bar 2, P
2represent secondary carborundum depression bar 2-1 pressure, S
2represent the area of the pressure face of secondary carborundum depression bar 2-1;
Pass through formula: P
1s
1=P
2s
2,
the diameter of the secondary carborundum depression bar 2-1 needed for calculating is 25.8mm; The internal diameter of three grades of graphite jig covers 1 is 10mm, and the internal diameter of secondary graphite jig cover 1-1 is 25.8mm;
(2) tungsten block is prepared:
Tungsten powder embodiment one prepared loads in the two-stage pressurizing device of driven dimension in (1), two-stage pressurizing device is loaded in vacuum discharge plasma sintering furnace, control sintering temperature 1200 DEG C, vacuum is 0.1Pa, sintering time 5 minutes, the pressure that forcing press gives secondary carborundum depression bar 2-1 is 90MPa;
As shown in Figure 4, obtaining tungsten block density is 93.92%, and average grain size is 620nm, and vickers microhardness is 676.45kg/mm
2.
Embodiment six: prepare tungsten block
With embodiment five unlike sintering time 10 minutes;
As shown in Figure 5: obtaining tungsten block density is 96.6%, and average grain size is 783nm, and vickers microhardness is 631kg/mm
2.
Embodiment seven: prepare tungsten block
With embodiment five unlike sintering temperature 1300 DEG C, sintering time 10 minutes;
As shown in Figure 6: the tungsten block density obtained is 97.2%, and average grain size is 1.16 μm, and vickers microhardness is 546kg/mm
2.
Embodiment eight: prepare tungsten block
With embodiment five unlike: control sintering temperature 1400 DEG C, sintering time 5 minutes;
As shown in Figure 7: the tungsten block density obtained is 97.8%, and average grain size is 1.35 μm, and vickers microhardness is 536kg/mm
2.
Claims (10)
1. a pressure head, the axis of this pressure head is the direction of exerting pressure of pressure head, it is characterized in that, described pressure head is axially arranged with at least two-stage along it, wherein away from treating that the one-level of pressure-like product is far-end level, the material of this far-end level is graphite, and treats that the material of the one-level that pressure-like product directly contact is carborundum.
2. pressure head as claimed in claim 1, is characterized in that, the diameter edge at different levels of described pressure head is away from treating that the direction of pressure-like product increases successively.
3. pressure head as claimed in claim 2, it is characterized in that, on described pressure head, material is the level of graphite is graphite linings, and material is the level of carborundum is silicon carbide layer, wherein: between adjacent graphite linings and silicon carbide layer, be provided with silicon carbide plate, and the diameter of silicon carbide plate is identical with the diameter of graphite linings.
4. a pressue device, is characterized in that, this pressue device comprises pressure head described in claim 1,2 or 3 and graphite jig cover, and the far-end level of described pressure head is electrically connected between overlapping with graphite jig.
5. pressue device as claimed in claim 4, it is characterized in that, described graphite jig cover comprises at least two-stage, is provided with the corresponding stage of pressure head in graphite jig cover at different levels.
6. pressure head according to claim 1 is for the preparation of the application of rare metal.
7. pressue device according to claim 4 is for the preparation of the application of rare metal.
8. the application described in claim 7 or 8, is characterized in that, described rare metal is tungsten.
9. apply as claimed in claim 8, it is characterized in that, described application comprise particle diameter be 50 ~ 100nm tungsten powder pressure be 300MPa ~ 1GPa, temperature carries out sintering obtained tungsten block under be 1200 ~ 1500 DEG C and vacuum being the condition of 0.1Pa, the time wherein sintered is 3 ~ 15min.
10. apply as claimed in claim 9, it is characterized in that, the density of described tungsten block is 93% ~ 99%, and the crystallite dimension of tungsten block is 0.6 ~ 1.5 μm, and the vickers microhardness of tungsten block is 520 ~ 680kg/mm
2.
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| CN106694897A (en) * | 2016-12-27 | 2017-05-24 | 中国兵器科学研究院宁波分院 | Method for preparing tungsten-based high-density alloy nano-composite powder and block material made of nano-composite powder |
| CN109755143A (en) * | 2017-11-01 | 2019-05-14 | 天津环鑫科技发展有限公司 | A kind of silicon slice alloy technique |
| CN112091211A (en) * | 2020-08-20 | 2020-12-18 | 上海交通大学 | Preparation method of diffusion multi-element joint |
| CN113927032A (en) * | 2021-09-02 | 2022-01-14 | 山东晶盾新材料科技有限公司 | Mold structure for rapid hot-pressing sintering |
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| WO2006113354A2 (en) * | 2005-04-15 | 2006-10-26 | The Regents Of The University Of California | Dense nanostructured oxides with fine crystals prepared by field activation sintering |
| US20090072700A1 (en) * | 2007-09-18 | 2009-03-19 | Nichia Corporation | Phosphor-containing molded member, method of manufacturing the same, and light emitting device having the same |
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| CN106694897A (en) * | 2016-12-27 | 2017-05-24 | 中国兵器科学研究院宁波分院 | Method for preparing tungsten-based high-density alloy nano-composite powder and block material made of nano-composite powder |
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| CN113927032A (en) * | 2021-09-02 | 2022-01-14 | 山东晶盾新材料科技有限公司 | Mold structure for rapid hot-pressing sintering |
| CN113927032B (en) * | 2021-09-02 | 2022-09-16 | 山东晶盾新材料科技有限公司 | Mold structure for rapid hot-pressing sintering |
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Application publication date: 20150422 |