CN105798295B - A kind of preparation method of molybdenum and molybdenum alloy part - Google Patents

A kind of preparation method of molybdenum and molybdenum alloy part Download PDF

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CN105798295B
CN105798295B CN201610164589.8A CN201610164589A CN105798295B CN 105798295 B CN105798295 B CN 105798295B CN 201610164589 A CN201610164589 A CN 201610164589A CN 105798295 B CN105798295 B CN 105798295B
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molybdenum
powder
mixed
molybdenum alloy
alloy part
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CN105798295A (en
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薛蕾
赵晓明
王俊伟
杨东辉
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Xian Bright Laser Technologies Co Ltd
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Xian Bright Laser Technologies Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F12/00Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
    • B22F12/40Radiation means
    • B22F12/41Radiation means characterised by the type, e.g. laser or electron beam
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102Metallic powder coated with organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10Formation of a green body
    • B22F10/16Formation of a green body by embedding the binder within the powder bed
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/12Both compacting and sintering
    • B22F3/14Both compacting and sintering simultaneously
    • B22F3/15Hot isostatic pressing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B33ADDITIVE MANUFACTURING TECHNOLOGY
    • B33YADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
    • B33Y10/00Processes of additive manufacturing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10Processes characterised by the sequence of their steps
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency

Abstract

The invention discloses the preparation methods of a kind of molybdenum and molybdenum alloy part, include the following steps:Molybdenum powder or molybdenum alloy powder are taken, itself and rare earth element powder mixed-powder is mixed to get, then organic adhesive is added under the conditions of being protected from light in mixed-powder and is uniformly mixed, then adds antifoaming agent and defoam to obtain mixed slurry;Mixed slurry is fitted into 3D printing former, is successively printed according to three-dimensional part model by the way of face exposure or spot scan using controllable UV Line beam, molybdenum or molybdenum alloy part crude green body is made;Crude green body is subjected to low-temperature defatted processing and hip treatment, obtains fine and close molybdenum or molybdenum alloy part.This method utilizes 3D printing rapid shaping principle, and the shape of part is unfettered, simplifies process, shortens the manufacturing cycle, and product compactness is preferable.

Description

A kind of preparation method of molybdenum and molybdenum alloy part
Technical field
The invention belongs to technical field of material, and in particular to the preparation method of a kind of molybdenum and molybdenum alloy part.
Background technology
(1100~1650 DEG C) have high intensity at high temperature for molybdenum or molybdenum alloy, are easily worked compared with tungsten, thus in electricity Son pipe (grid and anode), electric light source (backing material), metal working tools (die casting and extrusion die and perforating head) manufacture It is applied in department and aerospace industry.Molybdenum is resistant to the etch of melten glass, its oxide will not pollute glass.From 1943 Since year, molybdenum materials makees heating electrode for glass industry always.Mo-30W alloys have the performance of excellent resist melt zine corrosion, It has been applied successfully to zinc metallurgy industry.Molybdenum is additionally operable to the components such as heat exchanger and valve in manufacture gas washing in SA production.Molybdenum alloy Manufacture generally by being crushed coarse as-cast grain in technologies such as 1100~1400 DEG C of temperature range hot extrusions, forging, rollings, Improve the processing performance of ingot casting, obtain tubing, bar, plank, proximate matter etc., complex structure product is added by machinery after hot working The method of work obtains final product structure.
The forming of existing molybdenum or molybdenum alloy part is generally realized using the method for plastic processing, and the strong of molybdenum alloy can be improved Spend and improve its cold plasticity.Molybdenum and molybdenum alloy can use conventional plastic processing method to produce plank, band, foil, tubing, stick Material, wire rod and proximate matter.The characteristics of molybdenum alloy material is processed, which is per pass thermal deformation manufacturing procedure, obviously product final performance Influence.Molybdenum aoxidizes sharply above at 600 DEG C, volatilizees in 725 DEG C or so oxidation products and liquid phase, therefore molybdenum and its alloy occurs Generally use hydrogen or the protection of other reducing atmospheres when heating.The ingot blank of molybdenum and its alloy is mainly produced with powder metallurgical technique, Also it can be produced with smelting technology.General small dimension blank mostly uses powder metallurgical technique, both big specification blank can be used.
The shortcomings that method made above is:1) since molybdenum has the deficiencies of black brittleness, intensity is low, ductility is poor, molybdenum is closed Gold progress deep processing is relatively difficult, and application is by larger limitation.2) machinery is generally required after traditional heat processing technique processing to add Work, stock utilization is low, and the manufacturing cycle is long, and heat processing technique is difficult to accurately control;3) prior powder metallurgy technique needs to make Particular manufacturing craft, die cost is high, and the period is long;4) existing powder metallurgy is only capable of being simple to manufacture molybdenum with heat processing technique technology or molybdenum closes Golden infrastructure product.Disadvantage mentioned above makes mould heat pressure sintering method not be suitable for small lot and complicated shape molybdenum or molybdenum alloy part Production.
Invention content
The object of the present invention is to provide the preparation methods of a kind of molybdenum and molybdenum alloy part, solve existing mold hot pressed sintering side Method is not suitable for the problem of small lot and complicated shape molybdenum or production of molybdenum alloy part.
The technical solution adopted in the present invention is, the preparation method of a kind of molybdenum and molybdenum alloy part includes the following steps:
Step 1, prepared by raw material
Molybdenum powder or molybdenum alloy powder are taken, it is mixed to get with rare earth element powder to mixed-powder, then by mixed-powder Organic adhesive is added under the conditions of being protected from light to be uniformly mixed, then adds antifoaming agent mixing, surface is removed after bubble recession Impurity obtains mixed slurry.
Step 2, crude green body manufactures
Mixed slurry is fitted into 3D printing former, using controllable UV Line beam, using face exposure or spot scan Mode, successively printed according to three-dimensional part model, molybdenum or molybdenum alloy part crude green body be made.
Step 3, it post-processes
Molybdenum or molybdenum alloy part crude green body are subjected to low-temperature defatted processing, so that the organic adhesive in crude green body is evaporated and overflows;Again Hip treatment is carried out, fine and close molybdenum or molybdenum alloy part are obtained.
The features of the present invention also characterized in that:
Preferably, rare earth element powder is La, Y or Ce.
Preferably, in mixed-powder, rare earth element powder accounts for the 0.5%~1% of mixed-powder total volume, remaining is molybdenum powder End or molybdenum alloy powder.
Preferably, organic adhesive is epoxy acrylic resin, unsaturated polyester resin, urethane acrylate, polyester One of acrylate, polyester acrylate resin or amino acrylic resin.
Antifoaming agent can be used as lower alcohol, organically-modified compound, organic polymer, organic siliconresin, mineral oil etc..It is excellent Select ethyl alcohol, n-butanol, tributyl phosphate, metallic soap, polyethers, polyacrylate, polydimethyl siloxane fluid or modified polyorganosiloxane it One.
Preferably, the volume ratio of mixed-powder and organic adhesive is 3:7~3:2, antifoaming agent accounts for mixed slurry total volume 0.05%~1.0%.
Preferably, for the layer thickness control successively printed at 20~80 μm, optical source wavelength is 200~400nm.
Preferably, when being exposed using face, time for exposure 0.1-3s;When using spot scan, spot diameter be 0.1~ 0.15mm, hot spot movement speed 1-300mm/min.
Preferably, 200 DEG C~400 DEG C of the temperature of low-temperature defatted processing, time 2-4h.
Preferably, 1250 DEG C~1400 DEG C of hip treatment temperature, pressure 100MPa~200MPa, time 2-5h.
Preferably, molybdenum alloy is molybdenum and tungsten alloy, molybdenum-copper, molybdenum hafnium carbon alloy, vitallium or titanium-zirconium-molybdenum alloy.
The invention has the advantages that the present invention utilizes 3D printing technique manufacture molybdenum and molybdenum alloy part, the shape of part It is unfettered, the defect that must use mold in existing manufacturing technology is avoided, process is simplified, shortens the manufacturing cycle, improve Molybdenum or molybdenum alloy part manufacture efficiency.By adding the rare earth element of certain content in molybdenum or molybdenum alloy powder, refinement is brilliant Grain purifies crystal boundary and changes Grain boundary morphology, to improve the plasticity of molybdenum under the high temperature conditions.
Specific implementation mode
The present invention is described in further detail With reference to embodiment, but the present invention is not limited to these realities Apply mode.
The present invention provides the preparation method of a kind of molybdenum and molybdenum alloy part, this method can be used for preparing pure molybdenum part, It can be used for preparing molybdenum alloy part.Molybdenum alloy include molybdenum and tungsten alloy, molybdenum-copper, molybdenum hafnium carbon alloy, vitallium or Titanium-zirconium-molybdenum alloy etc..Specific preparation method is as follows:
Step 1, prepared by raw material
99%~99.5% molybdenum powder or molybdenum alloy powder are taken according to volume ratio, is mixed with 0.5%~1% rare earth powder Mixed-powder is obtained, then organic adhesive is added in mixed-powder and is sufficiently mixed.The preferred epoxy acrylic tree of organic adhesive Fat, unsaturated polyester resin, urethane acrylate, polyester acrylate, polyester acrylate resin or amino acrylic resin. The volume ratio of mixed-powder and organic adhesive is 3:7~3:2.To ensure the good mobility of slurry, mixed process and storage Process should avoid light-exposed, particularly avoid ultraviolet light, mixed process avoids being mixed into excessive impurity oxygen as possible, it is ensured that high temperature sintering Quality.
Molybdenum powder or molybdenum alloy powder are added rare earth element and can be purified crystal boundary with crystal grain thinning and changed Grain boundary morphology, from And improve the moulding of molybdenum.Rare earth powder preferred La, Y or Ce.
In order to reduce the bubble generated in whipping process, antifoaming agent is added in above-mentioned mixed liquor, is slowly stirred, to reduce Surface tension of liquid around bubble makes small bubble coalescence at big bubble, finally makes bubbles burst, plays and suppress or eliminate The effect of bubble in slurry.After slurry air entrapment recession, pulp surface floating material or residue are removed, obtains uniform bubble-free Mixed slurry.Lower alcohol, organically-modified compound, mineral oil, organic polymer, organic siliconresin etc. can be selected in antifoaming agent, Preferred alcohol, n-butanol, tributyl phosphate, metallic soap, polyethers, polyacrylate, polydimethyl siloxane fluid or modified polyorganosiloxane One of, addition accounts for the 0.05%~1.0% of mixed slurry total volume.
Step 2, crude green body manufactures
Mixed slurry is fitted into 3D printing former, using controllable UV Line beam, using face exposure or spot scan Mode, successively printed according to three-dimensional part model, molybdenum or molybdenum alloy part crude green body be made.The layer thickness control successively printed is 20 ~80 μm, optical source wavelength is 200~400nm.It is exposed according to face, time for exposure 0.1-3s;According to spot scan, hot spot is straight Diameter is 0.1~0.15mm, and hot spot movement speed is 1-300mm/min.
Step 3, it post-processes
In order to reduce influence of the organic adhesive to molybdenum and molybdenum alloy mechanical property, molybdenum or molybdenum alloy part crude green body are existed Low-temperature defatted processing 2-4h is carried out at 200 DEG C~400 DEG C, so that the organic adhesive in crude green body is evaporated and is overflowed;Then, in order to obtain High-compactness part, then carry out hip treatment under the conditions of 1250 DEG C~1400 DEG C of temperature, pressure 100MPa~200MPa 2-5h obtains fine and close molybdenum or molybdenum alloy part.
The molybdenum or molybdenum alloy part consistency that the present invention prepares are higher, stable quality, high to the utilization rate of raw material, and And manufacturing speed is fast, especially complex, the especially fine part of energy forming shape is suitble to small lot production.
Embodiment 1
A kind of preparation method of pure molybdenum part, specifically includes following steps:
(1) prepared by raw material
The synthesis of unsaturated polyester resin:Unsaturated dibasic acid is using maleic acid and fumaric acid 1:1 mixing, while being added one Quantitative phthalic anhydride, succinic acid can improve the elasticity of unsaturated polyester (UP), reduce volume contraction, increase the modeling of polyester Property.Dihydric alcohol uses ethylene glycol.
The specific synthesis technology of unsaturated polyester resin is:Unsaturated dibasic acid, dihydric alcohol and suitable polymerization inhibitor are added Enter into reactor, be passed through nitrogen, stirring is warming up to 160 DEG C of reflux, survey acid value to 200mgKOH/g or so, starts to be discharged, and rises Temperature is to 175~200 DEG C, when acid value reaches setting value, stops reaction, is cooled to 80 DEG C or so, and 20%~30% activity is added Diluent (styrene or esters of acrylic acid reactive diluent) and the discharging of appropriate polymerization inhibitor.Wherein, unsaturated dibasic acid uses horse Carry out sour and fumaric acid with 1:1 mass ratio mixes, while the elasticity of phthalic anhydride and succinic acid improvement unsaturated polyester (UP) is added, Volume contraction is reduced, the plasticity of polyester is increased.Dihydric alcohol uses ethylene glycol.
99% pure molybdenum powder (grain size is 50 μm) is taken according to volume ratio, the La powder with 1% is mixed to get mixed-powder, then Unsaturated polyester resin is added under the conditions of being protected from light in mixed-powder and is sufficiently mixed, mixed-powder and unsaturated polyester resin body Product is than being 3:7.Then antifoaming agent ethyl alcohol is added thereto, is slowly stirred, after slurry air entrapment recession, removes pulp surface Floating material or residue obtain the mixed slurry of uniform bubble-free;Antifoaming agent accounts for the 0.05% of mixed slurry total volume.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, in such a way that face exposes, root are utilized It is successively printed according to three-dimensional part model, thickness is 20 μm, optical source wavelength 200nm, time for exposure 3s and molybdenum part is successively made Crude green body.
(3) it post-processes
By in made molybdenum part crude green body merging low-temperature sintering stove, low-temperature defatted processing 4h is carried out at 200 DEG C, is made organic Bonding agent overflows, volatilizees.Again by the molybdenum part crude green body merging hot isostatic pressing stove after degreasing, at 1250 DEG C, 150MPa, carry out Hip treatment 4h obtains fine and close pure molybdenum part.
Embodiment 2
A kind of preparation method of pure molybdenum part, specifically includes following steps:
(1) prepared by raw material
99.5% pure molybdenum powder (grain size is 50 μm) is taken according to volume ratio, the Y powder with 0.5% is mixed to get mixed powder End, then epoxy acrylic resin is added under the conditions of being protected from light in mixed-powder and is sufficiently mixed, mixed-powder and epoxy acrylic Resin volume ratio is 3:5.Then antifoaming agent metallic soap is added thereto, is slowly stirred, after slurry air entrapment recession, removal Pulp surface floating material or residue obtain the mixed slurry of uniform bubble-free;Antifoaming agent accounts for the 0.05% of mixed slurry total volume.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, by the way of spot scan, root are utilized It is successively printed according to three-dimensional part model, thickness is 80 μm, optical source wavelength 400nm, spot diameter 0.1mm, hot spot movement speed 1mm/min is spent, tungsten part crude green body is successively made.
(3) it post-processes
By in made molybdenum part crude green body merging low-temperature sintering stove, low-temperature defatted processing 3h is carried out at 400 DEG C, is made organic Bonding agent overflows, volatilizees.Again by the molybdenum part crude green body merging hot isostatic pressing stove after degreasing, at 1300 DEG C, 200MPa, carry out Hip treatment 3h obtains fine and close pure molybdenum part.
Embodiment 3
A kind of preparation method of molybdenum and tungsten alloy part, specifically includes following steps:
(1) prepared by raw material
According to volume ratio take 99% molybdenum and tungsten alloy powder, 1% Ce powder be mixed to get mixed-powder, then by mixed-powder Epoxy acrylic resin is added under the conditions of being protected from light and is sufficiently mixed, mixed-powder is 1 with epoxy acrylic resin volume ratio:1. Then antifoaming agent tributyl phosphate is added thereto, is slowly stirred, after slurry air entrapment recession, removal pulp surface floating Object or residue obtain the mixed slurry of uniform bubble-free;Antifoaming agent accounts for the 0.5% of mixed slurry total volume.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, in such a way that face exposes, root are utilized It is successively printed according to three-dimensional part model, thickness is 80 μm, optical source wavelength 400nm, time for exposure 3s, and the conjunction of molybdenum tungsten is successively made Metal parts crude green body.
(3) it post-processes
By in made molybdenum and tungsten alloy part crude green body merging low-temperature sintering stove, low-temperature defatted processing 3h is carried out at 300 DEG C, Organic adhesive is set to overflow, volatilization.Again by after degreasing molybdenum and tungsten alloy part crude green body merging hot isostatic pressing stove in, 1350 DEG C, Under 200MPa, hip treatment 2h is carried out, obtains fine and close molybdenum and tungsten alloy part.
Embodiment 4
A kind of preparation method of molybdenum hafnium carbon alloy part, specifically includes following steps:
(1) prepared by raw material
The molybdenum alloy powder containing hafnium 1.0% (mass fraction), carbon 0.05%~0.08% (mass fraction) is taken, according still further to body Product ratio takes the 99% molybdenum hafnium carbon alloy powder and 1% La powder to be mixed to get mixed-powder, then mixed-powder is being protected from light item Polyester acrylate is added under part and is sufficiently mixed, mixed-powder is 3 with polyester acrylate volume ratio:2.Then add thereto Enter antifoaming agent tributyl phosphate, be slowly stirred, after slurry air entrapment recession, removes pulp surface floating material or residue, obtain Obtain the mixed slurry of uniform bubble-free;Antifoaming agent accounts for the 1% of mixed slurry total volume.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, by the way of spot scan, root are utilized It is successively printed according to three-dimensional part model, thickness is 20 μm, optical source wavelength 300nm, spot diameter 0.15mm, hot spot movement speed 150mm/min is spent, molybdenum hafnium carbon alloy part crude green body is successively made.
(3) it post-processes
By in made molybdenum hafnium carbon alloy part crude green body merging low-temperature sintering stove, low-temperature defatted processing is carried out at 400 DEG C 3h makes organic adhesive overflow, volatilization.The molybdenum hafnium carbon alloy part crude green body after degreasing is placed in hot isostatic pressing stove again, 1400 DEG C, under 110MPa, carry out hip treatment 2h, obtain fine and close molybdenum hafnium carbon alloy part.
Embodiment 5
A kind of preparation method of titanium-zirconium-molybdenum alloy part, specifically includes following steps:
(1) prepared by raw material
Take the titanium zirconium molybdenum of titaniferous 1.25% (mass fraction), zirconium 0.15% (mass fraction), carbon 0.15% (mass fraction) Alloy powder takes the 99.5% titanium-zirconium-molybdenum alloy powder and 0.5%Ce powder to be mixed to get mixed-powder according still further to volume ratio, then Amino acrylic resin is added under the conditions of being protected from light in mixed-powder and is sufficiently mixed, mixed-powder and amino acrylic resin body Product is than being 3:7.Then antifoaming agent polydimethyl siloxane fluid is added thereto, is slowly stirred, after slurry air entrapment recession, removal Pulp surface floating material or residue obtain the mixed slurry of uniform bubble-free;Antifoaming agent accounts for the 1% of mixed slurry total volume.
(2) crude green body manufactures
Mixed slurry is fitted into 3D printing former, controllable UV Line beam, by the way of spot scan, root are utilized It is successively printed according to three-dimensional part model, thickness is 50 μm, optical source wavelength 200nm, spot diameter 0.1mm, hot spot movement speed 150mm/min is spent, niobium tungsten alloy part crude green body is successively made.
(3) it post-processes
By in made titanium-zirconium-molybdenum alloy part crude green body merging low-temperature sintering stove, low-temperature defatted processing is carried out at 400 DEG C 2h makes organic adhesive overflow, volatilization.The titanium-zirconium-molybdenum alloy part crude green body after degreasing is placed in hot isostatic pressing stove again, 1400 DEG C, under 100MPa, carry out hip treatment 5h, obtain fine and close titanium-zirconium-molybdenum alloy part.
The compactness and toughness of molybdenum and molybdenum alloy part that 1-5 of the embodiment of the present invention is prepared are good, can meet market Product demand, it is also different, can meet the needs of different shape part.
For the present invention using 3D printing technique manufacture molybdenum and molybdenum alloy part, the shape of part is unfettered, avoids existing system The defect of mold must be used by making in technology, simplified process, shortened the manufacturing cycle, and molybdenum or the manufacture of molybdenum alloy part are improved Efficiency.
Above description of the present invention is section Example, and but the invention is not limited in above-mentioned embodiment. Above-mentioned specific implementation mode is schematical, is not restrictive.Every material using the present invention and method are not taking off In the case of present inventive concept and scope of the claimed protection, it is all it is specific expansion belong to protection scope of the present invention it It is interior.

Claims (7)

1. the preparation method of a kind of molybdenum and molybdenum alloy part, which is characterized in that include the following steps:
Step 1, prepared by raw material
Molybdenum powder or molybdenum alloy powder are taken, itself and rare earth element powder are mixed to get mixed-powder, then mixed-powder is being kept away Organic adhesive is added under the conditions of light to be uniformly mixed, then adds antifoaming agent mixing, surface impurity is removed after bubble recession, Obtain mixed slurry;
The rare earth element powder is La, Y or Ce;The rare earth element powder accounts for the 0.5%~1% of mixed-powder total volume, Remaining is the molybdenum powder or molybdenum alloy powder;
The organic adhesive is unsaturated polyester resin;
The specific synthesis technology of the unsaturated polyester resin is:Unsaturated dibasic acid, dihydric alcohol and polymerization inhibitor are added to instead It answers in device, is passed through nitrogen, stirring is warming up to 160 DEG C of reflux, and survey acid value starts to be discharged to 200mgKOH/g, it is warming up to 175~ 200 DEG C, when acid value reaches setting value, stops reaction, be cooled to 80 DEG C, 20%~30% reactive diluent and polymerization inhibitor is added Discharging;
The volume ratio of the mixed-powder and the organic adhesive is 3:7~3:2, it is total that the antifoaming agent accounts for the mixed slurry The 0.05%~1.0% of volume;
Step 2, crude green body manufactures
Mixed slurry is fitted into 3D printing Stereolithography equipment, using controllable UV Line beam, is exposed or is put using face and swept The mode retouched successively is printed according to three-dimensional part model, and molybdenum or molybdenum alloy part crude green body is made;
Step 3, it post-processes
Molybdenum or molybdenum alloy part crude green body are subjected to low-temperature defatted processing, so that the organic adhesive in crude green body is evaporated and overflows;It carries out again Hip treatment obtains fine and close molybdenum or molybdenum alloy part.
2. the preparation method of molybdenum according to claim 1 and molybdenum alloy part, which is characterized in that the antifoaming agent is second Alcohol, n-butanol, tributyl phosphate, metallic soap, polyethers, polyacrylate, polydimethyl siloxane fluid or modified polyorganosiloxane.
3. the preparation method of molybdenum according to claim 1 and molybdenum alloy part, which is characterized in that the layer successively printed At 20~80 μm, optical source wavelength is 200~400nm for thickness control.
4. the preparation method of molybdenum according to claim 1 and molybdenum alloy part, which is characterized in that the printing type uses When face exposes, time for exposure 0.1-3s;When the printing type uses spot scan, spot diameter is 0.1~0.15mm, hot spot Movement speed 1-300mm/min.
5. the preparation method of molybdenum according to claim 1 and molybdenum alloy part, which is characterized in that the low-temperature defatted processing 200 DEG C~400 DEG C of temperature, time 2-4h.
6. the preparation method of molybdenum according to claim 1 and molybdenum alloy part, which is characterized in that the hip treatment 1250 DEG C~1400 DEG C of temperature, pressure 100MPa~200MPa, time 2-5h.
7. the preparation method of the molybdenum and molybdenum alloy part according to any one of claim 1-6, which is characterized in that the molybdenum Alloy is molybdenum and tungsten alloy, molybdenum-copper, molybdenum hafnium carbon alloy, vitallium or titanium-zirconium-molybdenum alloy.
CN201610164589.8A 2016-03-22 2016-03-22 A kind of preparation method of molybdenum and molybdenum alloy part Active CN105798295B (en)

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