CN104889392A - Material increasing manufacturing method of pure tungsten metal - Google Patents
Material increasing manufacturing method of pure tungsten metal Download PDFInfo
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- CN104889392A CN104889392A CN201510201677.6A CN201510201677A CN104889392A CN 104889392 A CN104889392 A CN 104889392A CN 201510201677 A CN201510201677 A CN 201510201677A CN 104889392 A CN104889392 A CN 104889392A
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Abstract
The invention relates to a material increasing manufacturing method of pure tungsten metal. The manufacturing method comprises steps of taking ball-shaped pure tungsten powder particles; screening out and mixing tungsten powder small particles and tungsten powder big particles to obtain mixed powder bodies; installing a metal substrate on an optical fiber laser work bench; filling a powder body stock bin with the mixed powder bodies and sealing a shaping cavity body; using a vacuum pump to pump the interior of the shaping cavity body to be in vacuum degree of -90Kpa; inputting protection gas into the shaping cavity body; repeating vacuumization and protection gas inputting so as to allow the oxygen content in the shaping cavity body to be reduced to less than 300ppm; scanning the sacrificing area of the metal substrate with laser until the oxygen content is reduced to less than 50ppm; sending the mixed powder bodies in the powder body stock bin to the metal substrate by a powder laying machine; using a powder laying scraper to lay the powder bodies so as to obtain a mixed powder body thin layer; fusing the mixed powder bodies in a shaping slicing area via high-energy laser beams; refusing the mixed powder bodies after each layer is shaped; after the refusing is finished, reducing the work bench by one slice thickness; and repeating the laser shaping and refusing until the whole part is finally shaped.
Description
Technical field
The present invention relates to a kind of increasing material manufacture method of pure tungsten metal, belong to and increase material manufacture field.
Background technology
Pure tungsten is a kind of refractory metal, has the characteristics such as high-melting-point, high density, elevated temperature strength and high rigidity, is widely used in the fields such as Aero-Space, national defence weapon, fusion energy resource.But because the fusing point of tungsten is high, forming property is poor, founding, powder metallurgy, injection moulding, plasma spraying can only be adopted at present shaping to its processing, these method complex process, need expensive moulds of industrial equipment, and can only the simple part of shaping opposed configuration.
Increasing material manufacture is a kind of New Processing, is different from traditional " removal type " and manufactures, do not need proembryo and mould, directly according to the electronic 3-D model data of part, formed the object of any complicated shape by the method successively increasing material.Increasing material manufacture for materials such as titanium alloy, stainless steel, nickel-base alloys is studied, and carries out more both at home and abroad, also comparatively ripe at present.But for refractory metal and alloy, such as tungsten, molybdenum, tantalum, vanadium etc., be subject to the intrinsic physical property impact such as its fusing point, density, thermal conductance, melt tension and viscosity, mainly there is the shortcomings such as molten drop instability, spherodization is remarkable, density is not high, increase material manufacture difficulty very large, its technological process control is studied also less both at home and abroad.Material manufacture is increased for tungsten, research both domestic and external is mostly for tungsten alloy, as W-Fe, W-Ni, W-Cu etc., Fe, Ni or Cu melt under Source as adhesives, and by unfused tungsten particle parcel wherein and mutually bonding, be typical liquid sintering process, this can reduce the shaping difficulty of tungsten alloy.
Compared with tungsten alloy, pure tungsten is shaping must based on fusing/process of setting completely, due to the fusing point of tungsten and thermal conductance all higher, under Source molten drop to sprawl/solidify behavior comparatively complicated, be difficult to realize densification completely, therefore the increasing material forming technological process control of pure tungsten does not obtain breakthrough always.
Summary of the invention
The increasing material that technical problem to be solved by this invention is to provide a kind of pure tungsten metal manufactures (3D printing) method, the present invention is based on precinct laser fusion (Selective Laser Melting, or powder bed lf SLM), special preprocess method and process measure is adopted to ensure the compact formed of pure tungsten metal, its novelty is under series of processes measure ensures, reduce pure tungsten and increase material forming defects, improve density.
The present invention is based on existing selective laser fusing (Selective Laser Melting, or powder bed lf equipment SLM), its cardinal principle is in substrate, lay certain thickness metal powder layer (being generally 20 μm ~ 100 μm) in advance, then high energy thermal source (laser or electron beam) is utilized to melt according to computer chip formation and profile track the powder thin layer being in loose condition (of surface) laid in advance, melt by high energy thermal source irradiation zone/solidify, other region powder still keep not melting state and play certain follow-up supporting function.By repeating the mode successively spreading powder, successively consolidation is piled up, can shaping arbitrary shape high-compactness 3 d part.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of increasing material manufacture method of pure tungsten metal, comprising:
1) screening and proportioning tungsten powder granule
In order to improve final molding density, first the bulk density improving pure tungsten powder granule is needed, and the bulk density of pure tungsten powder granule is subject to intergranular friction, grain shape, liquid fiber surface interaction and the impact of the factor such as granularity, distribution, pure tungsten powder granule is therefore needed to be spherical
Get the spherical pure tungsten powder granule of surperficial free from admixture and oxygen desorption, filter out tungsten powder body bulky grain and tungsten powder body granule, the oarse-grained median particle diameter of tungsten powder body is 15-20 μm, the short grained median particle diameter of tungsten powder body is 1-3 μm, tungsten powder body granule and the oarse-grained fineness ratio of tungsten powder body (tungsten powder body granule diameter ratio oarse-grained with tungsten powder body) are 0.1-0.2
Tungsten powder body granule is mixed (two yardstick) with tungsten powder body bulky grain; obtain mixed powder; the oarse-grained quality of tungsten powder body accounts for the 65%-75% of mixed powder quality; the short grained quality of tungsten powder body accounts for the 35%-25% of mixed powder quality; thus meet certain domain size distribution (bimodal distribution); now tungsten powder body bulky grain is main body; tungsten powder body granule embeds in the space between tungsten powder body bulky grain; the solid density of pine dress bulk density>=50% of mixed powder; solid density is element physical quantity, and the solid density of pure tungsten is 19.3g/cm
3, pine dress bulk density refers to that powder filling is when measuring vessel, does not apply the density measured by any external force.Method of testing according to the mensuration of GB/T1479.1-2011 metal dust apparent density, part 1: funnel method perform.
In mixed powder, add calcium, rare earth element and carbon black, the quality adding calcium is no more than 1.5% of mixed powder quality, and the quality adding rare earth element is no more than 1.5% of mixed powder quality, and the quality adding carbon black is no more than 0.5% of mixed powder quality,
2) laser formation and remelting
Selective laser melt-forming is ordinary skill in the art means, but prior art can't use selective laser melt-forming tungsten metal, in order to overcome the high thermal conductance of tungsten, high-melting-point, high melt viscosity, high melt tension characteristic, the application passes through particle diameter ratio and the mass ratio of screening and proportioning globular tungsten powder body particle, add molten bath stable element, optimize optical fiber laser parameter, scanning strategy and powder bed parameter, and adopt laser remolten, the special process measure such as preheating and novel " MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate ", overcome this technology barrier, the innovative point of the application that Here it is.
The step of selective laser melt-forming and remelting comprises:
A, on the workbench of optical fiber laser, metal substrate is installed, and metal substrate is preheated to 200-600 DEG C, the gap simultaneously controlling paving powder scraper and metal substrate is 30 μm, in laser formation and reflow process, metal substrate remains at 200-600 DEG C, by 1) mixed powder prepared is filled in powder material warehouse;
B, seal molding cavity, will be evacuated to relative vacuum degree for-90KPa (relative experimental ground atmospheric pressure, this patent experiment place is Beijing) with vavuum pump in shaped cavity;
C, to input protection gases argon, nitrogen or helium in shaped cavity;
D, repetition B-C step, oxygen content in shaped cavity is made to be down to below 300ppm, then with laser, metal substrate " sacrifice region " is scanned, consume residual oxygen in molding cavity, until oxygen content is down to below 50ppm, carrying out strict Control for Oxygen Content to molding cavity, is to avoid the oxidation in forming process and strong unusual thermocapillary convection phenomenon as far as possible, thus reduce molten drop reunion nodularization, improve final molding density;
E, the mixed powder sent on metal substrate by Pu Fen mechanism in powder material warehouse, and paved by paving powder scraper, obtain the mixed powder thin layer of thickness 30 μm;
F, start shaping, by the mixed powder in high energy laser beam melt-forming break area, in 30min, in molding cavity, oxygen content is down to < 1ppm, and in laser formation and reflow process oxygen content < 1ppm all the time in molding cavity;
Remelting again after G, each mixed powder thin layer are shaping, namely do not spread mixed powder laser to rescan once (laser remelting), surface roughness is reduced, lower one deck paving powder is more even, and improve final density, scanning direction and the shaping scanning direction angle of laser remolten are 90 °, to reduce overall residual stress, as shown in Figure 1-2;
After H, remelting complete, workbench declines a slice thickness (mixed powder thickness of thin layer) 30 μm;
I, repetition step e-H, until whole part forming is complete.
On the basis of technique scheme, the present invention can also do following improvement.
Further, 1) in, described rare earth element is one or more in lanthanide series lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium.
Adopting the beneficial effect of this step to be that to add lanthanide series be nodularization problem in order to suppress the oxidation in forming process and strong thermocapillary convection to cause, strengthening laser absorption.
Further, 2) A in, described metal substrate is MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate, preparation method is as follows: get 316L corrosion resistant plate (Renishaw companies market product), installing hole is being had near 316L corrosion resistant plate edge, for being connected with the workbench of former, 316L corrosion resistant plate is slotted, single groove area is no more than 100cm
2, the degree of depth is no more than 5mm, asbestos are positioned in groove, as thermal insulation layer, get the tungsten plate matched with groove shape, to be positioned in groove on asbestos, between tungsten plate and corrosion resistant plate, bonding or screw is fixed, tungsten plate surface and 316L corrosion resistant plate surface are at grade, MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate is divided into sacrifice region and shaped cut sheets region, shaped cut sheets region is the region at tungsten plate place in MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate, sacrifice region is the region in MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate outside tungsten plate, as seen in figs. 5-6.
The beneficial effect of this step is adopted to be in order to avoid other elements are to the pollution of tungsten, shaping substrate adopts rolling tungsten plate, but because the thermal conductance of tungsten plate is higher, laser heat can be transferred away rapidly, therefore MULTILAYER COMPOSITE steel-heat-barrier material-tungsten substrate must be adopted, reduce overall thermal conductance, reduce laser heat loss, avoid steel contaminating impurity tungsten.
Further, 2) A in, when described mixed powder is filled into powder material warehouse, need to carry out in the glove box under argon shield, mixed powder cross after, when being again filled into powder material warehouse, also need to carry out under argon shield.
The beneficial effect of this step is adopted to be avoid powder adsorb oxygen.
Further, 2) G in, if do not form the fusing track that mutually overlap joint is good after laser remolten scanning, then repeat 2-3 remelting, the situation of satisfaction is as Fig. 3, and unsatisfied situation is as Fig. 4.
Further, 2) in, described laser formation is consistent with the parameter of remelting or inconsistent, the parameter of described laser formation is the power output > 400W of optical fiber laser, Laser output is modulating pulse zlasing mode, in order to stabilised bath, Laser output is modulating pulse zlasing mode, spot diameter < 100 μm, point is apart from (point distance) 30-50 μm, time for exposure (exposure time) 200-300 μ s, speed 150-200mm/s, sweep span (Hatch space) 80-120 μm, consider that tungsten powder body is to the absorption coefficient of laser, after the factors such as reflection, practical laser power density > 3 × 10
6w/cm
2,
The parameter of described laser remolten is the power output > 400W of optical fiber laser, Laser output is modulating pulse zlasing mode, spot diameter < 100 μm, point is apart from 30-50 μm, time for exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 10
6w/cm
2
It is the key factor ensureing shaping density that laser and sweep parameter are arranged:
Due to employing is modulating pulse laser pulse, speed (speed)=distance (point the distance)/time for exposure (exposure time), therefore, point distance (point distance) is 30-50 μm of selection, time for exposure (exposure time) is selected at 200-300 μ s, and according to pulverulence overall balance, regulate the speed at 150-200mm/s, as shown in Figure 7.
Adjust each parameter, the ratio of the enthalpy change (Δ H) that material absorbing laser energy is produced and material fusion enthalpy (Hs) is at 3-7.
ΔH＝(ω·P)/(π·(α·v·d
3)
0.5)
Hs＝(κ·T
m)/α
ω: laser absorption rate, P: laser energy, α: thermal diffusion coefficient, v: laser speed, d: spot diameter;
The invention has the beneficial effects as follows:
The invention provides a kind of increasing material manufacture method of pure tungsten metal, ensure by adopting globular tungsten powder body ratio optimization and shaping process measures, solve pure tungsten metal and increase during material manufactures the problems such as the molten drop state labile, nodularization, the defect hole that exist be more, improve shaping density and component capabilities, after this method process, test tungsten compact density reach 18g/cm
3above, relative density more than 93%.
Accompanying drawing explanation
Fig. 1 is the scan pattern of laser formation of the present invention;
Fig. 2 is that the scanning direction of laser formation of the present invention and the scanning direction angle of remelting are 90 ° and scheme;
Fig. 3 forms the fusing trajectory diagram that overlap joint is good mutually after laser remolten of the present invention scanning;
Fig. 4 does not form the fusing trajectory diagram that overlap joint is good mutually after laser remolten of the present invention scanning;
Fig. 5 is the structural representation of MULTILAYER COMPOSITE of the present invention iron-heat-barrier material-tungsten substrate;
Fig. 6 is the structural representation of MULTILAYER COMPOSITE of the present invention iron-heat-barrier material-tungsten substrate;
Fig. 7 is the structural representation of laser parameter of the present invention adjustment;
Fig. 8 is the structural representation of pure tungsten small-sized products prepared by embodiment 1;
Fig. 9 is the structural representation of tokamak device pure tungsten divertor module prepared by embodiment 2;
Figure 10 is the micro-organization chart of tokamak device pure tungsten divertor module prepared by embodiment 2;
Figure 11 is the structural representation of pure tungsten grid prepared by embodiment 3;
In accompanying drawing, the list of parts representated by each label is as follows:
1, shaped cut sheets region, 2, tungsten plate, 3,316L corrosion resistant plate, 4, sacrifice region, 5, installing hole, 6, asbestos, 7, pulse laser point distance, 8, sweep span.
Detailed description of the invention
Be described principle of the present invention and feature below, example, only for explaining the present invention, is not intended to limit scope of the present invention.
Embodiment of the present invention globular tungsten powder body used particle is bought from refractory material branch company of AT&M, adopts TEKNA induction plasma powder nodularization device processes.
In embodiment, device therefor is the selective laser melt-forming equipment of Renishaw company.
In embodiment, 316L corrosion resistant plate used is Renishaw companies market product.
Embodiment 1
1) screening and proportioning tungsten powder granule
Get the spherical pure tungsten powder granule of surperficial free from admixture and oxygen desorption, filter out tungsten powder body bulky grain and tungsten powder body granule, the oarse-grained median particle diameter of tungsten powder body is 18.3 μm, and the short grained median particle diameter of tungsten powder body is 2.1 μm, tungsten powder body granule and the oarse-grained fineness ratio of tungsten powder body are 0.11
Mixed with tungsten powder body bulky grain by tungsten powder body granule, obtain mixed powder, the oarse-grained quality of tungsten powder body accounts for 70% of mixed powder quality, and the short grained quality of tungsten powder body accounts for 30% of mixed powder quality, and the pine dress bulk density of mixed powder is 53%.
In mixed powder, add La and carbon black, the quality adding La is 0.3% of mixed powder quality, and the quality adding carbon black is 0.3% of mixed powder quality,
2) laser formation and remelting
A, on workbench, install MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate, be preheated to 300 DEG C and keep this temperature in laser formation and reflow process, the gap of paving powder scraper and MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate is 30 μm; In the glove box of argon shield, by 1) mixed powder prepared is filled in powder material warehouse.
Described MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base plate preparation method is as follows: get 316L corrosion resistant plate 3,316L corrosion resistant plate 3 edge and have installing hole 5, for being connected with the workbench of optical fiber laser.316L corrosion resistant plate 3 opens rectangular channel, single groove area 50cm
2(10cm × 5cm), degree of depth 5mm, be positioned in groove by same size asbestos 6, thickness is 3mm (can compress), as thermal insulation layer, get the tungsten plate (thickness 3mm) 2 matched with groove shape, be positioned in groove on asbestos 6, be screwed between tungsten plate 2 and 316L corrosion resistant plate 3, adjustment bolt tightening dynamics, make tungsten plate 2 surface and 316L corrosion resistant plate 3 surface at grade, as Fig. 5-6.
B, seal molding cavity, being evacuated to relative vacuum degree is-90KPa, input protection gases argon in shaped cavity; Repeatedly vacuumize and input protection gases argon, make oxygen content in shaped cavity be down to below 300ppm.
C, with laser, MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate " sacrifice region 4 " to be scanned, consume residual oxygen in molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent on MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate by D, Pu Fen mechanism, and is paved by paving powder scraper, obtains the mixed powder thin layer of thickness 30 μm;
E, start shaping, by the mixed powder of high energy laser beam melt-forming break area 1, in 30min, in molding cavity, oxygen content is down to < 1ppm, and in laser formation and reflow process oxygen content < 1ppm all the time in molding cavity; Laser power is greater than 400W, some distance 50 μm, time for exposure 250 μ s, sweep span 100 μm.
F, do not spread mixed powder, laser rescans remelting.Scanning direction and the shaping scanning direction angle of laser remolten are 90 °; Parameter is identical with E.
After G, remelting complete, workbench declines a slice thickness 30 μm;
H, repetition step e-G, until whole part forming is complete, obtain pure tungsten fritter, as Fig. 8, tungsten compact density reaches 18g/cm
3above, relative density more than 93%.
Embodiment 2
1) screening and proportioning tungsten powder granule
Get the spherical pure tungsten powder granule of surperficial free from admixture and oxygen desorption, filter out tungsten powder body bulky grain and tungsten powder body granule, the oarse-grained median particle diameter of tungsten powder body is 18.3 μm, and the short grained median particle diameter of tungsten powder body is 2.1 μm, tungsten powder body granule and the oarse-grained fineness ratio of tungsten powder body are 0.11
Mixed with tungsten powder body bulky grain by tungsten powder body granule, obtain mixed powder, the oarse-grained quality of tungsten powder body accounts for 70% of mixed powder quality, and the short grained quality of tungsten powder body accounts for 30% of mixed powder quality, and the pine dress bulk density of mixed powder is 53%.
In mixed powder, add La and carbon black, the quality adding La is 0.3% of mixed powder quality, and the quality adding carbon black is 0.3% of mixed powder quality,
2) laser formation and remelting
A, on workbench, install MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate, be preheated to 300 DEG C and keep this temperature in laser formation and reflow process, the gap of paving powder scraper and MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate is 30 μm; In the glove box of argon shield, by 1) mixed powder prepared is filled in powder material warehouse.
Described MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base plate preparation method is as follows: get 316L corrosion resistant plate 3,316L corrosion resistant plate 3 edge and have installing hole 5, for being connected with the workbench of optical fiber laser.316L corrosion resistant plate 3 opens rectangular channel, single groove area 50cm
2(10cm × 5cm), degree of depth 5mm, be positioned in groove by same size asbestos 6, thickness is 3mm (can compress), as thermal insulation layer, get the tungsten plate 2 (thickness 3mm) matched with groove shape, be positioned in groove on asbestos 6, be screwed between tungsten plate 2 and 316L corrosion resistant plate 3, adjustment bolt tightening dynamics, make tungsten plate 2 surface and 316L corrosion resistant plate 3 surface at grade, as Fig. 5-6.
B, seal molding cavity, being evacuated to relative vacuum degree is-90KPa, input protection gases argon in shaped cavity; Repeatedly vacuumize and input protection gases argon, make oxygen content in shaped cavity be down to below 300ppm.
C, with laser, MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate " sacrifice region 4 " to be scanned, consume residual oxygen in molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent on MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate by D, Pu Fen mechanism, and is paved by paving powder scraper, obtains the mixed powder thin layer of thickness 30 μm;
E, start shaping, by the mixed powder of high energy laser beam melt-forming break area 1, in 30min, in molding cavity, oxygen content is down to < 1ppm, and in laser formation and reflow process oxygen content < 1ppm all the time in molding cavity; Laser power is greater than 400W, some distance 50 μm, time for exposure 280 μ s, sweep span 110 μm.
F, do not spread mixed powder, laser rescans remelting.Scanning direction and the shaping scanning direction angle of laser remolten are 90 °; Parameter is identical with E.
After G, remelting complete, workbench declines a slice thickness 30 μm;
H, repetition step e-G, until whole part forming is complete, obtain tokamak device pure tungsten divertor module verification part, as Fig. 9, and compact density 18g/cm
3above, thermal conductivity 70-90W/mK, microstructure is as Figure 10.
Embodiment 3
1) screening and proportioning tungsten powder granule
Get the spherical pure tungsten powder granule of surperficial free from admixture and oxygen desorption, filter out tungsten powder body bulky grain and tungsten powder body granule, the oarse-grained median particle diameter of tungsten powder body is 18.3 μm, and the short grained median particle diameter of tungsten powder body is 2.1 μm, tungsten powder body granule and the oarse-grained fineness ratio of tungsten powder body are 0.11
Mixed with tungsten powder body bulky grain by tungsten powder body granule, obtain mixed powder, the oarse-grained quality of tungsten powder body accounts for 70% of mixed powder quality, and the short grained quality of tungsten powder body accounts for 30% of mixed powder quality, and the pine dress bulk density of mixed powder is 53%.
In mixed powder, add La and carbon black, the quality adding La is 0.3% of mixed powder quality, and the quality adding carbon black is 0.3% of mixed powder quality,
2) laser formation and remelting
A, on workbench, install MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate, be preheated to 300 DEG C and keep this temperature in laser formation and reflow process, the gap of paving powder scraper and MULTILAYER COMPOSITE iron-heat-barrier material-tungsten substrate is 30 μm; In the glove box of argon shield, by 1) mixed powder prepared is filled in powder material warehouse.
Described MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base plate preparation method is as follows: get 316L corrosion resistant plate 3,316L corrosion resistant plate 3 edge and have installing hole 5, for being connected with the workbench of optical fiber laser.316L corrosion resistant plate 3 opens rectangular channel, single groove area 50cm
2(10cm × 5cm), degree of depth 5mm, be positioned in groove by same size asbestos 6, thickness is 3mm (can compress), as thermal insulation layer, get the tungsten plate 2 (thickness 3mm) matched with groove shape, be positioned in groove on asbestos 6, be screwed between tungsten plate 2 and 316L corrosion resistant plate 3, adjustment bolt tightening dynamics, make tungsten plate 2 surface and 316L corrosion resistant plate 3 surface at grade, as Fig. 5-6.
B, seal molding cavity, being evacuated to relative vacuum degree is-90KPa, input protection gases argon in shaped cavity; Repeatedly vacuumize and input protection gases argon, make oxygen content in shaped cavity be down to below 300ppm.
C, with laser, MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate " sacrifice region 4 " to be scanned, consume residual oxygen in molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent on MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate by D, Pu Fen mechanism, and is paved by paving powder scraper, obtains the mixed powder thin layer of thickness 30 μm;
E, start shaping, by the mixed powder of high energy laser beam melt-forming break area 1, in 30min, in molding cavity, oxygen content is down to < 1ppm, and in laser formation and reflow process oxygen content < 1ppm all the time in molding cavity; Laser power is greater than 400W, some distance 50 μm, time for exposure 230 μ s, sweep span 90 μm.
F, do not spread mixed powder, laser rescans remelting.Scanning direction and the shaping scanning direction angle of laser remolten are 90 °; Parameter is identical with E.
After G, remelting complete, workbench declines a slice thickness 30 μm;
H, repetition step e-G, until whole part forming is complete, obtain pure tungsten grid, as Figure 11, and overall dimensions 10mm*10mm*3mm, aperture 0.1mm.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. an increasing material manufacture method for pure tungsten metal, is characterized in that, comprising:
1) screening and proportioning tungsten powder granule
Get the spherical pure tungsten powder granule of surperficial free from admixture and oxygen desorption, filter out tungsten powder body bulky grain and tungsten powder body granule, the oarse-grained median particle diameter of tungsten powder body is 15-20 μm, the short grained median particle diameter of tungsten powder body is 1-3 μm, tungsten powder body granule and the oarse-grained fineness ratio of tungsten powder body are 0.1-0.2
Tungsten powder body granule is mixed with tungsten powder body bulky grain; obtain mixed powder, the oarse-grained quality of tungsten powder body accounts for the 65%-75% of mixed powder quality, and the short grained quality of tungsten powder body accounts for the 35%-25% of mixed powder quality; the solid density of pine dress bulk density >=50% of mixed powder
In mixed powder, add calcium, rare earth element and carbon black, the quality adding calcium is no more than 1.5% of mixed powder quality, and the quality adding rare earth element is no more than 1.5% of mixed powder quality, and the quality adding carbon black is no more than 0.5% of mixed powder quality,
2) laser formation and remelting
A, on the workbench of optical fiber laser, metal substrate is installed, and metal substrate is preheated to 200-600 DEG C, the gap simultaneously controlling paving powder scraper and metal substrate is 30 μm, in laser formation and reflow process, metal substrate remains at 200-600 DEG C, by 1) mixed powder prepared is filled in powder material warehouse;
B, seal molding cavity are-90KPa with vavuum pump by being evacuated to relative vacuum degree in shaped cavity;
C, to input protection gases argon, nitrogen or helium in shaped cavity;
D, repetition B-C step, make oxygen content in shaped cavity be down to below 300ppm, then scan metal substrate " sacrifice region " with laser, consumes residual oxygen in molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent on metal substrate by E, Pu Fen mechanism, and is paved by paving powder scraper, obtains the mixed powder thin layer of thickness 30 μm;
F, start shaping, by the mixed powder in high energy laser beam fusing " shaped cut sheets region ", in 30min, in molding cavity, oxygen content is down to < 1ppm, and in laser formation and reflow process oxygen content < 1ppm all the time in molding cavity;
Remelting again after G, each mixed powder thin layer are shaping, namely do not spread mixed powder laser and rescan once, scanning direction and the shaping scanning direction angle of laser remolten are 90 °;
After H, remelting complete, workbench declines a slice thickness 30 μm;
I, repetition step e-H, until whole part forming is complete.
2. increasing material manufacture method according to claim 1, is characterized in that, 1) in, described rare earth element is one or more in lanthanide series lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium.
3. increasing material manufacture method according to claim 1 and 2, it is characterized in that, 2) A in, described metal substrate is MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate, preparation method is as follows: get 316L corrosion resistant plate, is having installing hole, for being connected with the workbench of former near 316L corrosion resistant plate edge, 316L corrosion resistant plate is slotted, and single groove area is no more than 100cm
2, the degree of depth is no more than 5mm, is positioned over by asbestos in groove, as thermal insulation layer, gets the tungsten plate matched with groove shape, is positioned in groove on asbestos, and between tungsten plate and corrosion resistant plate, bonding or screw is fixed, and tungsten plate surface and 316L corrosion resistant plate surface are at grade.
4. increasing material manufacture method according to claim 3, is characterized in that, 2) A in, when described mixed powder is filled into powder material warehouse, need to carry out in the glove box under argon shield.
5. the increasing material manufacture method according to claim 1,2 or 4, it is characterized in that, 2) in, described laser formation is consistent with the parameter of remelting or inconsistent, the parameter of described laser formation is the power output > 400W of optical fiber laser, Laser output is modulating pulse zlasing mode, spot diameter < 100 μm, point is apart from 30-50 μm, time for exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 10
6w/cm
2;
The parameter of described laser remolten is the power output > 400W of optical fiber laser, Laser output is modulating pulse zlasing mode, spot diameter < 100 μm, point is apart from 30-50 μm, time for exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 10
6w/cm
2.
6. increasing material manufacture method according to claim 3, it is characterized in that, 2) in, described laser formation is consistent with the parameter of remelting or inconsistent, the parameter of described laser formation is the power output > 400W of optical fiber laser, Laser output is modulating pulse zlasing mode, spot diameter < 100 μm, point is apart from 30-50 μm, time for exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 10
6w/cm
2;
The parameter of described laser remolten is the power output > 400W of optical fiber laser, Laser output is modulating pulse zlasing mode, spot diameter < 100 μm, point is apart from 30-50 μm, time for exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 10
6w/cm
2.
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