CN104889392B - A kind of increasing material manufacture method of pure tungsten metal - Google Patents

A kind of increasing material manufacture method of pure tungsten metal Download PDF

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CN104889392B
CN104889392B CN201510201677.6A CN201510201677A CN104889392B CN 104889392 B CN104889392 B CN 104889392B CN 201510201677 A CN201510201677 A CN 201510201677A CN 104889392 B CN104889392 B CN 104889392B
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powder
tungsten
laser
mixed powder
quality
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CN201510201677.6A
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CN104889392A (en
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周鑫
沈志坚
刘伟
马静
王殿政
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清华大学
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Abstract

nullThe present invention relates to the increasing material manufacture method of a kind of pure tungsten metal,Including: take spherical pure tungsten powder granule,Sift out the little granule of tungsten powder body and tungsten powder body bulky grain,Mix to obtain mixed powder,Optical fiber laser work platforms is installed metal basal board,Mixed powder is filled in powder material warehouse,Seal molding cavity,It is 90Kpa with vacuum pump by being evacuated to relative vacuum degree in shaped cavity,Protective gas is inputted in shaped cavity,Repeat evacuation and input protective gas,In making shaped cavity, oxygen content is down to below 300ppm,With laser, metal basal board " sacrifice region " is scanned,Until oxygen content is down to below 50ppm,Mixed powder in powder material warehouse is sent on metal basal board by Pu Fen mechanism,Paved by paving powder scraper,Obtain mixed powder thin layer,By the mixed powder in high energy laser beam fusing " shaped cut sheets region ",Remelting after each formable layer,After remelting completes,Work platforms declines a slice thickness,Repeat laser formation and reflow step,Until whole part forming is complete.

Description

A kind of increasing material manufacture method of pure tungsten metal
Technical field
The present invention relates to the increasing material manufacture method of a kind of pure tungsten metal, belong to increasing material and 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, It is widely used in the fields such as Aero-Space, national defence weapon, fusion energy resource.But due to melting of tungsten Point high, forming property is poor, to its processing can only use at present founding, powder metallurgy, injection moulding, etc. Plasma spray molding etc., these method complex process, need expensive moulds of industrial equipment, and can only molding phase Part to simple in construction.
Increasing material manufacture is a kind of New Processing, is different from traditional " removal type " and manufactures, it is not necessary to Proembryo and mould, directly according to the electronic 3-D model data of part, by successively increasing the side of material Method forms the object of any complicated shape.Increasing material for materials such as titanium alloy, rustless steel, nickel-base alloys Manufacture research, carry out more both at home and abroad, the most ripe.But for refractory metal and alloy, Such as tungsten, molybdenum, tantalum, vanadium etc., intrinsic by its fusing point, density, thermal conductance, melt tension and viscosity etc. Physical property affects, and is primarily present the shortcomings such as molten drop is unstable, spherodization is notable, consistency is the highest, Increasing material manufacture difficulty very big, its technique and method are studied the most less both at home and abroad.For tungsten increases material manufacture, Research both domestic and external is mostly for tungsten alloy, such as W-Fe, W-Ni, W-Cu etc., Fe, Ni or Cu Melt under Source as adhesives, and unfused tungsten particle is wrapped up wherein and the most viscous Connecing, be typical liquid sintering process, this can reduce tungsten alloy molding difficulty.
Compared with tungsten alloy, pure tungsten molding must be based on being completely melt/process of setting, due to the fusing point of tungsten The highest with thermal conductance, under Source, the sprawling of molten drop/solidification behavior is complex, is difficulty with The finest and close, therefore increasing material moulding process and the method for pure tungsten does not obtains breakthrough always.
Summary of the invention
The technical problem to be solved is to provide the increasing material of a kind of pure tungsten metal and manufactures (3D printing) Method, the present invention is based on precinct laser fusion (Selective Laser Melting, SLM) or powder Bed lf, the densification of pure tungsten metal becomes to use special preprocess method to ensure with process measure Type, its novelty is under series of processes measure ensures, reduces pure tungsten and increases material forming defects, improves consistency.
The present invention based on existing selective laser melt (Selective Laser Melting, SLM) or Powder bed lf equipment, its cardinal principle is to lay certain thickness metal dust in advance in substrate Layer (usually 20 μm~100 μm), then utilizes high energy thermal source (laser or electron beam) according to calculating Machine chip formation and profile track melt the powder thin layer being in loose condition (of surface) laid in advance, by high energy heat Source irradiation zone melts/solidifies, other region powder still keep the state that do not melts and play certain after Continuous supporting function.By the way of repeating successively to spread powder, successively consolidation accumulation, can be with molding arbitrary shape High-compactness 3 d part.
The technical scheme is that the increasing material manufacturer of a kind of pure tungsten metal Method, including:
1) screening and proportioning tungsten powder granule
In order to improve final molding consistency, it is necessary first to improve the bulk density of pure tungsten powder granule, and The bulk density of pure tungsten powder granule by intergranular friction, grain shape, liquid fiber surface interaction and granularity, The factor impacts such as distribution, it is therefore desirable to pure tungsten powder granule is spherical,
Take surface free from admixture and the spherical pure tungsten powder granule of oxygen absorption, filter out tungsten powder body bulky grain and tungsten The little granule of powder body, the oarse-grained median particle diameter of tungsten powder body is 15-20 μm, tungsten powder body short grained intermediate value grain Footpath is 1-3 μm, the little granule of tungsten powder body and the oarse-grained fineness ratio of tungsten powder body (the little granule of tungsten powder body and tungsten powder Body oarse-grained diameter ratio) it is 0.1-0.2,
Little for tungsten powder body granule is mixed (double yardstick) with tungsten powder body bulky grain, obtains mixed powder, tungsten powder The oarse-grained quality of body accounts for the 65%-75% of mixed powder quality, and the short grained quality of tungsten powder body accounts for mixed powder The 35%-25% of weight, thus meet certain particle diameter distribution (bimodal distribution), now tungsten powder body is big Granule is main body, and the little granule of tungsten powder body embeds in the space between tungsten powder body bulky grain, the pine of mixed powder The solid density of dress bulk density >=50%, solid density is element physical quantity, and the solid density of pure tungsten is 19.3g/cm3, pine dress bulk density refers to that powder filling, in time measuring container, does not apply any external force and surveyed The density obtained.Method of testing according to the mensuration of GB/T1479.1-2011 metal dust apparent density, the 1st Part: funnel method performs.
In mixed powder, add calcium, rare earth element and white carbon black, add the quality of calcium less than mixed powder The 1.5% of quality, adds the quality of rare earth element less than the 1.5% of mixed powder quality, addition carbon black Quality less than mixed powder quality 0.5%,
2) laser formation and remelting
Selective laser melt-forming is ordinary skill in the art means, but prior art can't use laser Selective melting molding tungsten metal, in order to overcome highly thermally conductive, high-melting-point, the high melt viscosity of tungsten, high melt Tensile property, the application, by screening and the particle diameter ratio of proportioning globular tungsten powder body granule and mass ratio, adds Molten bath stable element, optimizes optical fiber laser parameter, scanning strategy and powder bed parameter, and uses laser weight The special process measure such as molten, preheating and novel " MULTILAYER COMPOSITE ferrum-heat-barrier material-tungsten substrate ", overcomes This technology barrier, here it is the innovative point of the application.
Selective laser melt-forming includes with the step of remelting:
A, metal basal board is installed on the work platforms of optical fiber laser, and metal basal board is preheated to 200-600 DEG C, the gap simultaneously controlling paving powder scraper and metal basal board is 30 μm, at laser formation and weight During Rong, metal basal board remains at 200-600 DEG C, by 1) mixed powder prepared is filled into powder In body feed bin;
B, seal molding cavity, will be evacuated to relative vacuum degree for-90KPa (phase with vacuum pump in shaped cavity To sample plot atmospheric pressure, this patent experiment place is Beijing);
C, in shaped cavity, input protective gas argon, nitrogen or helium;
D, repetition B-C step, in making shaped cavity, oxygen content is down to below 300ppm, then uses laser Metal basal board " sacrifice region " is scanned, consumes residual oxygen in molding cavity, until oxygen content fall To below 50ppm, molding cavity is carried out strict Control for Oxygen Content, be to avoid molding as far as possible Oxidation in journey and strong unusual thermocapillary convection phenomenon, thus reduce molten drop reunion nodularization, improve final Molding consistency;
E, on metal basal board, sent into the mixed powder in powder material warehouse by Pu Fen mechanism, and scraped by paving powder Cutter is paved, and obtains the mixed powder thin layer of thickness 30 μm;
F, beginning molding, by the mixed powder in high energy laser beam melt-forming break area, at 30min In, in molding cavity, oxygen content is down to < 1ppm, and in laser formation with reflow process in molding cavity Oxygen content < 1ppm all the time;
Remelting again after G, each mixed powder thin layer molding, does not the most spread mixed powder laser and rescans Once (laser remelting), making surface roughness reduce, next layer paving powder is more uniform, and carries High final consistency, the scanning direction of laser remolten is 90 ° with the scanning direction angle of molding, to reduce Overall residual stress, as shown in Figure 1-2;
After H, remelting complete, work platforms 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 be lanthanide series lanthanum, cerium, praseodymium, neodymium, promethium, samarium, One or more in europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutecium.
Addition lanthanide series is to suppress the oxidation in forming process to use this step to provide the benefit that The nodularization problem caused with strong thermocapillary convection, strengthens laser absorption.
Further, 2) A in, described metal basal board is MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " Substrate, preparation method is as follows: takes 316L corrosion resistant plate (Renishaw companies market product), is leaning on Closely 316L corrosion resistant plate edge has installing hole, for being connected with the work platforms of former, Slotting on 316L corrosion resistant plate, single groove area is less than 100cm2, the degree of depth is less than 5mm, by asbestos It is positioned in groove, as thermal insulation layer, takes the tungsten plate matched with groove shape, 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 with In one plane, MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate is divided into sacrifice region and shaped cut sheets district Territory, 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, such as Fig. 5-6 Shown in.
, in order to avoid the pollution to tungsten of other elements, shaping substrate uses to use this step to provide the benefit that Rolling tungsten plate, but owing to the thermal conductance of tungsten plate is higher, laser heat can be transferred away rapidly, it is therefore necessary to use MULTILAYER COMPOSITE steel-heat-barrier material-tungsten substrate, reduces overall thermal conductance, reduces laser heat and scatters and disappears, it is to avoid steel Impurity pollutes tungsten.
Further, 2) A in, when described mixed powder is filled into powder material warehouse, need at argon Glove box under Bao Hu is carried out, after mixed powder is crossed, when being again filled into powder material warehouse, also needs To carry out under argon shield.
Using this step to provide the benefit that avoids powder body to adsorb oxygen.
Further, 2) G in, if not forming good molten of mutually overlap joint after laser remolten scanning Change track, then repeat 2-3 remelting, satisfied situation such as Fig. 3, unsatisfied situation such as Fig. 4.
Further, 2) in, described laser formation is consistent or inconsistent with the parameter of remelting, described sharp The parameter of Seterolithography is the output > 400W of optical fiber laser, and laser is output as modulating pulse laser mould Formula, for stabilised bath, laser is output as modulating pulsed laser mode, spot diameter < 100 μm, point Away from (point distance) 30-50 μm, time of exposure (exposure time) 200-300 μ s, Speed 150-200mm/s, sweep span (Hatch space) 80-120 μm, it is considered to tungsten powder body is to swashing After the factors such as the absorptance of light, reflection, practical laser power density > 3 × 106W/cm2
The parameter of described laser remolten is the output > 400W of optical fiber laser, and laser is output as modulation Pulsed laser mode, spot diameter < 100 μm, put away from 30-50 μm, time of exposure 200-300 μ s, Speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 106W/cm2
Laser and sweep parameter arrange the key factor being to ensure that molding consistency:
Owing to using modulation pulse laser pulse, speed (speed)=away from (point distance) / time of exposure (exposure time), therefore, puts away from (point distance) in 30-50 μm Selecting, time of exposure (exposure time) selects at 200-300 μ s, and combines according to pulverulence Occlusal equilibration, regulates the speed at 150-200mm/s, as shown in Figure 7.
Adjust each parameter, make enthalpy change (Δ H) and melt material enthalpy (Hs) that absorbed laser energy produces Ratio at 3-7.
Δ H=(ω P)/(π (α v d3)0.5)
Hs=(κ Tm)
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 present invention provides the increasing material manufacture method of a kind of pure tungsten metal, by using globular tungsten powder body proportioning excellent Change and shaping process measures ensure, solve pure tungsten metal increase material manufacture present in molten drop state labile, The problems such as nodularization, defect hole are more, improve molding consistency and component capabilities, treated by the present method after Test tungsten compact density reaches 18g/cm3Above, relative density more than 93%.
Accompanying drawing explanation
Fig. 1 is the scan pattern of laser formation of the present invention;
Fig. 2 is the scanning direction of laser formation of the present invention and the scanning direction angle of remelting is 90 ° of figures;
Fig. 3 is the formation fusing trajectory diagram that mutually overlap joint is good after laser remolten of the present invention scanning;
Fig. 4 is not formed after laser remolten of the present invention scans mutually to overlap good fusing trajectory diagram;
Fig. 5 is the structural representation of MULTILAYER COMPOSITE of the present invention ferrum-heat-barrier material-tungsten substrate;
Fig. 6 is the structural representation of MULTILAYER COMPOSITE of the present invention ferrum-heat-barrier material-tungsten substrate;
Fig. 7 is the structural representation that laser parameter of the present invention adjusts;
Fig. 8 is the structural representation of the pure tungsten small-sized products of embodiment 1 preparation;
Fig. 9 is the structural representation of the tokamak device pure tungsten divertor module of embodiment 2 preparation;
Figure 10 is the micro-organization chart of the tokamak device pure tungsten divertor module of embodiment 2 preparation;
Figure 11 is the structural representation of the pure tungsten grid of embodiment 3 preparation;
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, peace Dress hole, 6, asbestos, 7, pulse laser point away from, 8, sweep span.
Detailed description of the invention
Principle and feature to the present invention are described below, and example is served only for explaining the present invention, and Non-for limiting the scope of the present invention.
Globular tungsten powder body granule used by the embodiment of the present invention is bought from refractory material branch company of AT&M, adopts Process with TEKNA induction plasma powder body nodularization equipment.
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
Take surface free from admixture and the spherical pure tungsten powder granule of oxygen absorption, filter out tungsten powder body bulky grain and tungsten The little granule of powder body, the oarse-grained median particle diameter of tungsten powder body is 18.3 μm, tungsten powder body short grained intermediate value grain Footpath is 2.1 μm, and the little granule of tungsten powder body and the oarse-grained fineness ratio of tungsten powder body are 0.11,
Being mixed with tungsten powder body bulky grain by little for tungsten powder body granule, obtain mixed powder, tungsten powder body is oarse-grained Quality accounts for the 70% of mixed powder quality, and the short grained quality of tungsten powder body accounts for the 30% of mixed powder quality, The pine dress bulk density of mixed powder is 53%.
In mixed powder, add La and white carbon black, add quality is mixed powder quality the 0.3% of La, Add quality is mixed powder quality the 0.3% of carbon black,
2) laser formation and remelting
A, on work platforms install MULTILAYER COMPOSITE ferrum-heat-barrier material-tungsten substrate, be preheated to 300 DEG C and Laser formation and reflow process keep this temperature, paving powder scraper and MULTILAYER COMPOSITE ferrum-heat-barrier material-tungstenio The gap of plate is 30 μm;In the glove box of argon shield, by 1) mixed powder prepared is filled into powder In body feed bin.
Described MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base plate preparation method is as follows: take 316L rustless steel Plate 3,316L corrosion resistant plate 3 edge has installing hole 5, for the work platforms with optical fiber laser Connect.316L corrosion resistant plate 3 is opened rectangular channel, single groove area 50cm2(10cm × 5cm), deeply Same size asbestos 6 are positioned in groove by degree 5mm, and thickness is 3mm (can compress), as heat insulation Layer, takes the tungsten plate (thickness 3mm) 2 matched with groove shape, is positioned in groove on asbestos 6, tungsten plate 2 And be screwed between 316L corrosion resistant plate 3, adjust Bolt Tightening Force degree, make tungsten plate 2 surface With 316L corrosion resistant plate 3 surface at grade, such as Fig. 5-6.
B, seal molding cavity, being evacuated to relative vacuum degree is-90KPa, inputs in shaped cavity Protective gas argon;Evacuation and input protective gas argon, make oxygen content in shaped cavity repeatedly It is down to below 300ppm.
C, with laser, MULTILAYER COMPOSITE ferrum-heat-barrier material-tungsten substrate " sacrifice region 4 " is scanned, disappears Residual oxygen in consumption molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent into MULTILAYER COMPOSITE ferrum-heat-barrier material-tungstenio by D, Pu Fen mechanism On plate, and paved by paving powder scraper, obtain the mixed powder thin layer of thickness 30 μm;
E, beginning molding, by the mixed powder of high energy laser beam melt-forming break area 1, at 30min In, in molding cavity, oxygen content is down to < 1ppm, and in laser formation with reflow process in molding cavity Oxygen content < 1ppm all the time;Laser power is more than 400W, o'clock away from 50 μm, time of exposure 250 μ s, sweeps Retouch spacing 100 μm.
F, not spreading mixed powder, laser rescans remelting.The scanning direction of laser remolten and molding Scanning direction angle is 90 °;Parameter is identical with E.
After G, remelting complete, work platforms declines slice thickness 30 μm;
H, repetition step E-G, until whole part forming is complete, obtain pure tungsten fritter, such as Fig. 8, tungsten Compact density reaches 18g/cm3Above, relative density more than 93%.
Embodiment 2
1) screening and proportioning tungsten powder granule
Take surface free from admixture and the spherical pure tungsten powder granule of oxygen absorption, filter out tungsten powder body bulky grain and tungsten The little granule of powder body, the oarse-grained median particle diameter of tungsten powder body is 18.3 μm, tungsten powder body short grained intermediate value grain Footpath is 2.1 μm, and the little granule of tungsten powder body and the oarse-grained fineness ratio of tungsten powder body are 0.11,
Being mixed with tungsten powder body bulky grain by little for tungsten powder body granule, obtain mixed powder, tungsten powder body is oarse-grained Quality accounts for the 70% of mixed powder quality, and the short grained quality of tungsten powder body accounts for the 30% of mixed powder quality, The pine dress bulk density of mixed powder is 53%.
In mixed powder, add La and white carbon black, add quality is mixed powder quality the 0.3% of La, Add quality is mixed powder quality the 0.3% of carbon black,
2) laser formation and remelting
A, on work platforms install MULTILAYER COMPOSITE ferrum-heat-barrier material-tungsten substrate, be preheated to 300 DEG C and Laser formation and reflow process keep this temperature, paving powder scraper and MULTILAYER COMPOSITE ferrum-heat-barrier material-tungstenio The gap of plate is 30 μm;In the glove box of argon shield, by 1) mixed powder prepared is filled into powder In body feed bin.
Described MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base plate preparation method is as follows: take 316L rustless steel Plate 3,316L corrosion resistant plate 3 edge has installing hole 5, for the work platforms with optical fiber laser Connect.316L corrosion resistant plate 3 is opened rectangular channel, single groove area 50cm2(10cm × 5cm), deeply Same size asbestos 6 are positioned in groove by degree 5mm, and thickness is 3mm (can compress), as heat insulation Layer, takes the tungsten plate 2 (thickness 3mm) matched with groove shape, is positioned in groove on asbestos 6, tungsten plate 2 And be screwed between 316L corrosion resistant plate 3, adjust Bolt Tightening Force degree, make tungsten plate 2 surface With 316L corrosion resistant plate 3 surface at grade, such as Fig. 5-6.
B, seal molding cavity, being evacuated to relative vacuum degree is-90KPa, inputs in shaped cavity Protective gas argon;Evacuation and input protective gas argon, make oxygen content in shaped cavity repeatedly It is down to below 300ppm.
C, with laser, MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate " sacrifice region 4 " is scanned, Consume residual oxygen in molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent into MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " by D, Pu Fen mechanism On substrate, and paved by paving powder scraper, obtain the mixed powder thin layer of thickness 30 μm;
E, beginning molding, by the mixed powder of high energy laser beam melt-forming break area 1, at 30min In, in molding cavity, oxygen content is down to < 1ppm, and in laser formation with reflow process in molding cavity Oxygen content < 1ppm all the time;Laser power is more than 400W, o'clock away from 50 μm, time of exposure 280 μ s, sweeps Retouch spacing 110 μm.
F, not spreading mixed powder, laser rescans remelting.The scanning direction of laser remolten and molding Scanning direction angle is 90 °;Parameter is identical with E.
After G, remelting complete, work platforms declines slice thickness 30 μm;
H, repetition step E-G, until whole part forming is complete, obtains tokamak device pure tungsten and partially filter Device module verification part, such as Fig. 9, compact density 18g/cm3Above, thermal conductivity 70-90W/mK, microcosmic Tissue is such as Figure 10.
Embodiment 3
1) screening and proportioning tungsten powder granule
Take surface free from admixture and the spherical pure tungsten powder granule of oxygen absorption, filter out tungsten powder body bulky grain and tungsten The little granule of powder body, the oarse-grained median particle diameter of tungsten powder body is 18.3 μm, tungsten powder body short grained intermediate value grain Footpath is 2.1 μm, and the little granule of tungsten powder body and the oarse-grained fineness ratio of tungsten powder body are 0.11,
Being mixed with tungsten powder body bulky grain by little for tungsten powder body granule, obtain mixed powder, tungsten powder body is oarse-grained Quality accounts for the 70% of mixed powder quality, and the short grained quality of tungsten powder body accounts for the 30% of mixed powder quality, The pine dress bulk density of mixed powder is 53%.
In mixed powder, add La and white carbon black, add quality is mixed powder quality the 0.3% of La, Add quality is mixed powder quality the 0.3% of carbon black,
2) laser formation and remelting
A, on work platforms install MULTILAYER COMPOSITE ferrum-heat-barrier material-tungsten substrate, be preheated to 300 DEG C and Laser formation and reflow process keep this temperature, paving powder scraper and MULTILAYER COMPOSITE ferrum-heat-barrier material-tungstenio The gap of plate is 30 μm;In the glove box of argon shield, by 1) mixed powder prepared is filled into powder In body feed bin.
Described MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base plate preparation method is as follows: take 316L rustless steel Plate 3,316L corrosion resistant plate 3 edge has installing hole 5, for the work platforms with optical fiber laser Connect.316L corrosion resistant plate 3 is opened rectangular channel, single groove area 50cm2(10cm × 5cm), deeply Same size asbestos 6 are positioned in groove by degree 5mm, and thickness is 3mm (can compress), as heat insulation Layer, takes the tungsten plate 2 (thickness 3mm) matched with groove shape, is positioned in groove on asbestos 6, tungsten plate 2 And be screwed between 316L corrosion resistant plate 3, adjust Bolt Tightening Force degree, make tungsten plate 2 surface With 316L corrosion resistant plate 3 surface at grade, such as Fig. 5-6.
B, seal molding cavity, being evacuated to relative vacuum degree is-90KPa, inputs in shaped cavity Protective gas argon;Evacuation and input protective gas argon, make oxygen content in shaped cavity repeatedly It is down to below 300ppm.
C, with laser, MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate " sacrifice region 4 " is scanned, Consume residual oxygen in molding cavity, until oxygen content is down to below 50ppm;
Mixed powder in powder material warehouse is sent into MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " by D, Pu Fen mechanism On substrate, and paved by paving powder scraper, obtain the mixed powder thin layer of thickness 30 μm;
E, beginning molding, by the mixed powder of high energy laser beam melt-forming break area 1, at 30min In, in molding cavity, oxygen content is down to < 1ppm, and in laser formation with reflow process in molding cavity Oxygen content < 1ppm all the time;Laser power is more than 400W, o'clock away from 50 μm, time of exposure 230 μ s, sweeps Retouch spacing 90 μm.
F, not spreading mixed powder, laser rescans remelting.The scanning direction of laser remolten and molding Scanning direction angle is 90 °;Parameter is identical with E.
After G, remelting complete, work platforms declines slice thickness 30 μm;
H, repeat step E-G, until whole part forming is complete, obtain pure tungsten grid, such as Figure 11, Overall dimensions 10mm*10mm*3mm, aperture 0.1mm.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the present invention Spirit and principle within, any modification, equivalent substitution and improvement etc. made, should be included in this Within bright protection domain.

Claims (5)

1. the increasing material manufacture method of a pure tungsten metal, it is characterised in that including:
1) screening and proportioning tungsten powder granule
Take surface free from admixture and the spherical pure tungsten powder granule of oxygen absorption, filter out tungsten powder body bulky grain and tungsten The little granule of powder body, the oarse-grained median particle diameter of tungsten powder body is 15-20 μm, tungsten powder body short grained intermediate value grain Footpath is 1-3 μm, and the little granule of tungsten powder body and the oarse-grained fineness ratio of tungsten powder body are 0.1-0.2,
Being mixed with tungsten powder body bulky grain by little for tungsten powder body granule, obtain mixed powder, tungsten powder body is oarse-grained Quality accounts for the 65%-75% of mixed powder quality, and the short grained quality of tungsten powder body accounts for mixed powder quality 35%-25%, the solid density of pine dress bulk density >=50% of mixed powder,
In mixed powder, add calcium, rare earth element and white carbon black, add the quality of calcium less than mixed powder The 1.5% of quality, adds the quality of rare earth element less than the 1.5% of mixed powder quality, addition carbon black Quality less than mixed powder quality 0.5%,
2) laser formation and remelting
A, metal basal board is installed on the work platforms of optical fiber laser, and metal basal board is preheated to 200-600 DEG C, the gap simultaneously controlling paving powder scraper and metal basal board is 30 μm, at laser formation and weight During Rong, metal basal board remains at 200-600 DEG C, by 1) mixed powder prepared is filled into powder In body feed bin, described metal basal board is MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate, and preparation method is such as Under: take 316L corrosion resistant plate, having installing hole near 316L corrosion resistant plate edge, for and become The work platforms of type equipment connects, and slots on 316L corrosion resistant plate, and single groove area is less than 100cm2, The degree of depth is less than 5mm, is positioned in groove by asbestos, as thermal insulation layer, takes the tungsten matched with groove shape Plate, is positioned in groove on asbestos, and between tungsten plate and corrosion resistant plate, bonding or screw is fixed, tungsten plate surface with 316L corrosion resistant plate surface 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 MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " base The region at tungsten plate place in plate, sacrifice region is tungsten plate in MULTILAYER COMPOSITE " steel-heat-barrier material-tungsten " substrate Outside region;
B, seal molding cavity, be-90KPa with vacuum pump by being evacuated to relative vacuum degree in shaped cavity;
C, in shaped cavity, input protective gas argon, nitrogen or helium;
D, repetition B-C step, in making shaped cavity, oxygen content is down to below 300ppm, then uses laser Metal basal board " sacrifice region " is scanned, consumes residual oxygen in molding cavity, until oxygen content fall To below 50ppm;
Mixed powder in powder material warehouse is sent on metal basal board by E, Pu Fen mechanism, and by paving powder scraper paving Flat, obtain the mixed powder thin layer of thickness 30 μm;
F, beginning molding, 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 becomes with reflow process at laser formation Oxygen content < 1ppm all the time in cavity;
Remelting again after G, each mixed powder thin layer molding, does not the most spread mixed powder laser and rescans Once, the scanning direction of laser remolten is 90 ° with the scanning direction angle of molding;
After H, remelting complete, work platforms declines slice thickness 30 μm;
I, repetition step E-H, until whole part forming is complete.
Increasing material manufacture method the most according to claim 1, it is characterised in that 1) in, described Rare earth element be lanthanide series lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, One or more in thulium, ytterbium, lutecium.
Increasing material manufacture method the most according to claim 1, it is characterised 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.
4. according to the increasing material manufacture method described in claim 1,2 or 3, it is characterised in that 2) In, described laser formation is consistent or inconsistent with the parameter of remelting, and the parameter of described laser formation is optical fiber The output > 400W of laser instrument, laser is output as modulating pulsed laser mode, spot diameter < 100 μm, point is away from 30-50 μm, time of exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 106W/cm2
The parameter of described laser remolten is the output > 400W of optical fiber laser, and laser is output as modulation Pulsed laser mode, spot diameter < 100 μm, put away from 30-50 μm, time of exposure 200-300 μ s, Speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 106W/cm2
Increasing material manufacture method the most according to claim 1, it is characterised in that 2) in, described Laser formation is consistent or inconsistent with the parameter of remelting, and the parameter of described laser formation is optical fiber laser Output > 400W, laser be output as modulate pulsed laser mode, spot diameter < 100 μm, put away from 30-50 μm, time of exposure 200-300 μ s, speed 150-200mm/s, sweep span 80-120 μm, Practical laser power density > 3 × 106W/cm2
The parameter of described laser remolten is the output > 400W of optical fiber laser, and laser is output as modulation Pulsed laser mode, spot diameter < 100 μm, put away from 30-50 μm, time of exposure 200-300 μ s, Speed 150-200mm/s, sweep span 80-120 μm, practical laser power density > 3 × 106W/cm2
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