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CN105506370A - Ce and Nd reinforced titanium alloy material - Google Patents

Ce and Nd reinforced titanium alloy material Download PDF

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Publication number
CN105506370A
CN105506370A CN201510936053.9A CN201510936053A CN105506370A CN 105506370 A CN105506370 A CN 105506370A CN 201510936053 A CN201510936053 A CN 201510936053A CN 105506370 A CN105506370 A CN 105506370A
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titanium alloy
powder
printing
laser
alloy material
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毛培
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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
    • B22F10/20Direct sintering or melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C14/00Alloys based on titanium
    • B22F1/0003
    • 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
    • B22F10/00Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/62Treatment of workpieces or articles after build-up by chemical means
    • 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
    • B22F10/60Treatment of workpieces or articles after build-up
    • B22F10/64Treatment of workpieces or articles after build-up by thermal means
    • 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
    • B22F3/24After-treatment of workpieces or articles
    • 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
    • B22F10/30Process control
    • B22F10/36Process control of energy beam parameters
    • 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
    • B22F12/46Radiation means with translatory movement
    • B22F12/48Radiation means with translatory movement in height, e.g. perpendicular to the deposition plane
    • 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
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/247Removing material: carving, cleaning, grinding, hobbing, honing, lapping, polishing, milling, shaving, skiving, turning the surface
    • 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
    • B22F3/24After-treatment of workpieces or articles
    • B22F2003/248Thermal after-treatment
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides a Ce and Nd reinforced titanium alloy material. The preparation method of the material comprises the steps of powder preparing, laser 3D printing, vacuum annealing and electrochemical polishing. Through the selection of elementary composition of a titanium alloy powder raw material, the tensile strength, the elongation percentage and the percentage reduction of area of titanium alloy are improved obviously; a 3D printing raw material with uniform components and relatively good granularity can be obtained by adopting a way of ball milling, sintering and ball milling again; the 3D printing technology is combined with vacuum annealing, and the performances of the titanium alloy after printing are improved; and due to the adoption of electrochemical polishing, the problem of relatively high roughness of a 3D printed end product is solved.

Description

A kind of Ce, Nd strengthen titanium alloy material
Technical field
The present invention relates to titanium alloy material field, specifically, relate to a kind of Ce, Nd and strengthen titanium alloy material.
Background technology
Titanium alloy have lightweight, high-strength, corrosion-resistant, without many outstanding advantages such as magnetic, have a wide range of applications in fields such as Aeronautics and Astronautics, navigation, automobile, chemical industry, biomedicines.But titanium alloy is compared with other common metal, and also have the deficiencies such as high, the difficult processing of price, F-SP complex component, adopts and go material mechanical workout mode not only processing difficulties, and wastage of material is serious.Castmethod is adopted to prepare that not only yield rate is low but also casting flaw is many and performance is not high.Prepared by employing forging method, can only prepare simple shape and the little component of deflection.
3D printing technique is a kind of accumulation manufacturing technology, and the mode namely by successively printing carrys out constructed object.It is a kind of based on digital model file, uses special wax material, powdery metal or plastics etc. can jointing material, manufactures three-dimensional body by the jointing material printed from level to level.Present stage, three-dimensional printer was used to manufacture a product, and the principle of 3D printer is that data and raw material are put in 3D printer, and machine can be created product from level to level according to program, and so circulation is until workpiece completes, then obtains molded part through aftertreatment.Different from traditional removal materials processing technology, be therefore also called and add manufacture.
The material adopting 3D printing shaping to obtain often due to the material selected different, shaping time the binding agent selected etc. incorrect and process parameter control is bad, can cause the defects such as the billet surface that obtains is fuzzy, buckling deformation, size distortion, step-like surface, microtexture defect, fragmentation, staggered floor, this is fatal harm for 3D printing technique for the manufacture of medical device.Although its performance can be improved to a certain extent by subsequent heat treatment, owing to easily forming thick tissue in heat treatment process, thus reduce mechanical property.In addition, the surfaceness printing titanium alloy product due to laser 3D is poor, and a lot of structural member surface roughness requirements is very strict, and therefore, the problem of product coarse rugosity is also need at present to be solved further.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of Ce, Nd and strengthening titanium alloy material, this material is that a kind of 3D of high strength low roughness prints titanium alloy material.The technical solution used in the present invention is: a kind of Ce, Nd Doped with Titanium alloy material, and the preparation method of described titanium alloy material comprises the following steps: powder preparation, laser 3D printing, vacuum annealing and electro-chemical polish step; Wherein, described powder preparation process is: first being carried out by Titanium Powder powder stock being milled to granularity is below 200 orders, then sinter, sintering temperature is 1180-1250 DEG C, and soaking time is 1-2.5h, obtain titanium alloy agglomerate, described sintering block is carried out ball milling again, under 200-250r/min rotating speed, ball milling 8-10 hour, finally filter out the alloy powder that granularity is 15-25 μm, print raw material using it as laser 3D.
The titanium alloy powder raw material packet of described powder preparation process is containing following elementary composition: Al:2.50-3.80%, Zn:0.05-0.15%, Zr:0.85-0.95%, Hf:0.20-0.40%, V:2.20-2.50%, Ge:0.15-0.45%, Nd:0.50-0.80%, Nb:0.40-0.60%, Ce:1.20-1.50%, surplus is Ti, and above-mentioned per-cent is mass percent.
In described laser 3D printing step, blank is prepared into by 3D printing technique, the scan mode that 3D prints adopts orthogonal scanning, laser processing parameter is: laser power 200-250W, sweep velocity is 1250-1350mm/s, by blank ultrasonic cleaning 10 ~ 15mins shaping for Laser Printing, dry base substrate at 120 ~ 150 DEG C.
In described vacuum annealing step, Heating temperature is 850-880 DEG C, and soaking time is 1 ~ 1.5h, and vacuum tightness is 1.0 × 10 -3~ 10 -4pa.
In described electro-chemical polish step, adopt electrochemical etching to carry out aftertreatment, obtain the finished product that surfaceness is 0.6 μm ~ 0.7 μm.
The tensile strength of described finished product is 800 ~ 850MPa, and unit elongation and relative reduction in area are respectively 20% and 18%.
Preferably, the titanium alloy powder raw material packet that prepared by described powder contains following elementary composition: Al:2.80%, Zn:0.15%, Zr:0.85%, Hf:0.40%, V:2.50%, Ge:0.35%, Nd:0.70%, Nb:0.50%, Ce:1.50%, surplus is Ti, and above-mentioned per-cent is mass percent.
Advantage of the present invention is: selected by the elemental composition of Titanium Powder powder stock, obviously improve the tensile strength of titanium alloy, unit elongation and relative reduction in area; Employing ball milling-sintering-mode of ball milling obtains uniform composition again, the good 3D of granularity prints raw material; 3D printing technique is combined with vacuum annealing, improves the titanium alloy performance after printing; And utilize electrochemical etching to solve the higher problem of 3D printout roughness.
Embodiment
Below in conjunction with embodiment and comparative example, the present invention is described in more detail.
Embodiment 1:
Being carried out by Titanium Powder powder stock being milled to granularity is below 200 orders, then sinter, sintering temperature is 1180 DEG C, soaking time is 1h, obtains titanium alloy agglomerate, and described sintering block is carried out ball milling again, under 200r/min rotating speed, ball milling 10 hours, finally filters out the alloy powder that granularity is 15 μm, prints raw material using it as laser 3D.Wherein, employing comprises following elementary composition raw material as above-mentioned Titanium Powder powder stock: Al:2.80%, Zn:0.15%, Zr:0.85%, Hf:0.40%, V:2.50%, Ge:0.35%, Nd:0.70%, Nb:0.50%, Ce:1.50%, surplus is Ti, and above-mentioned per-cent is mass percent.Be prepared into blank by 3D printing technique, adopt orthogonal scanning, laser processing parameter is: laser power 200W, and sweep velocity is 1250mm/s, by blank ultrasonic cleaning 10mins shaping for Laser Printing, dries base substrate at 120 DEG C.Vacuum annealing step Heating temperature is 850 DEG C, and soaking time is 1h, and vacuum tightness is 1.0 × 10 -3pa.Adopt electrochemical etching to carry out aftertreatment, obtain the finished product that surfaceness is 0.6 μm.The tensile strength of finished product is 850MPa, and unit elongation and relative reduction in area are respectively 20% and 18%.
Embodiment 2:
Being carried out by Titanium Powder powder stock being milled to granularity is below 200 orders, then sinter, sintering temperature is 1250 DEG C, soaking time is 2.5h, obtains titanium alloy agglomerate, and described sintering block is carried out ball milling again, under 250r/min rotating speed, ball milling 8 hours, finally filters out the alloy powder that granularity is 25 μm, prints raw material using it as laser 3D.Wherein, employing comprises following elementary composition raw material as above-mentioned Titanium Powder powder stock: Al:2.50%, Zn:0.05%, Zr:0.95%, Hf:0.20%, V:2.20%, Ge:0.15%, Nd:0.50%, Nb:0.40%, Ce:1.20%, surplus is Ti, and above-mentioned per-cent is mass percent.Be prepared into blank by 3D printing technique, adopt orthogonal scanning, laser processing parameter is: laser power 250W, and sweep velocity is 1350mm/s, by blank ultrasonic cleaning 15mins shaping for Laser Printing, dries base substrate at 150 DEG C.Vacuum annealing step Heating temperature is 880 DEG C, and soaking time is 1.5h, and vacuum tightness is 1.0 × 10 -4pa.Adopt electrochemical etching to carry out aftertreatment, obtain the finished product that surfaceness is 0.7 μm.The tensile strength of finished product is 800MPa, and unit elongation and relative reduction in area are respectively 20% and 18%.
Embodiment 3:
Being carried out by Titanium Powder powder stock being milled to granularity is below 200 orders, then sinter, sintering temperature is 1200 DEG C, soaking time is 2h, obtains titanium alloy agglomerate, and described sintering block is carried out ball milling again, under 230r/min rotating speed, ball milling 9 hours, finally filters out the alloy powder that granularity is 20 μm, prints raw material using it as laser 3D.Wherein, employing comprises following elementary composition raw material as above-mentioned Titanium Powder powder stock: Al:3.80%, Zn:0.10%, Zr:0.90%, Hf:0.30%, V:2.30%, Ge:0.25%, Nd:0.60%, Nb:0.60%, Ce:1.30%, surplus is Ti, and above-mentioned per-cent is mass percent.Be prepared into blank by 3D printing technique, adopt orthogonal scanning, laser processing parameter is: laser power 220W, and sweep velocity is 1300mm/s, by blank ultrasonic cleaning 12mins shaping for Laser Printing, dries base substrate at 130 DEG C.Vacuum annealing step Heating temperature is 860 DEG C, and soaking time is 1h, and vacuum tightness is 1.0 × 10 -3pa.Adopt electrochemical etching to carry out aftertreatment, obtain the finished product that surfaceness is 0.6 μm.The tensile strength of finished product is 830MPa, and unit elongation and relative reduction in area are respectively 20% and 18%.
Comparative example 1:
To be undoped rare earth element ce and Nd, the Titanium Powder powder stock that other constituent contents are identical with embodiment 1, after adopting same powder preparation, laser 3D printing, vacuum annealing and electro-chemical polish step, the tensile strength of the titanium alloy product obtained is only up to 600MPa.
Comparative example 2:
By copper alloy identical with embodiment 1 with content for elemental composition, adopt the preparation of same powder, laser 3D printing and electro-chemical polish step, but change the processing parameter of vacuum annealing process, when Heating temperature is too high or too low, the tensile strength of its titanium alloy product obtained is the highest only has 500MPa, and unit elongation is 15%.
As can be seen from embodiment 1-3 and comparative example 1 and 2, titanium alloy material is strengthened according to a kind of Ce, Nd of the embodiment of the present invention by utilizing, selected by the elemental composition of Titanium Powder powder stock, obviously improve the tensile strength of titanium alloy, unit elongation and relative reduction in area; Employing ball milling-sintering-mode of ball milling obtains uniform composition again, the good 3D of granularity prints raw material; 3D printing technique is combined with vacuum annealing, improves the titanium alloy performance after printing; And utilize electrochemical etching to solve the higher problem of 3D printout roughness.
Although illustrate and describe embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple change, amendment, replacement and modification to these embodiments when not departing from principle of the present invention and aim, scope of the present invention is by claim and equivalents thereof.

Claims (7)

1. Ce, Nd strengthen a titanium alloy material, it is characterized in that: the preparation technology that described titanium alloy material adopts comprises the following steps: powder preparation, laser 3D printing, vacuum annealing and electro-chemical polish step; Wherein, described powder preparation process is: first being carried out by Titanium Powder powder stock being milled to granularity is below 200 orders, and then sinter, sintering temperature is 1180-1250 DEG C, and soaking time is 1-2.5h, obtains titanium alloy agglomerate; Described sintering block is carried out ball milling again, and under 200-250r/min rotating speed, ball milling 8-10 hour, finally filters out the alloy powder that granularity is 15-25 μm, prints raw material using it as laser 3D.
2. titanium alloy material according to claim 1, it is characterized in that: the titanium alloy powder raw material packet of described powder preparation process is containing following elementary composition: Al:2.50-3.80%, Zn:0.05-0.15%, Zr:0.85-0.95%, Hf:0.20-0.40%, V:2.20-2.50%, Ge:0.15-0.45%, Nd:0.50-0.80%, Nb:0.40-0.60%, Ce:1.20-1.50%, surplus is Ti, and above-mentioned per-cent is mass percent.
3. titanium alloy material according to claim 1, it is characterized in that: in described laser 3D printing step, blank is prepared into by 3D printing technique, the scan mode that 3D prints adopts orthogonal scanning, laser processing parameter is: laser power 200-250W, sweep velocity is 1250-1350mm/s, by blank ultrasonic cleaning 10 ~ 15mins shaping for Laser Printing, dries base substrate at 120 ~ 150 DEG C.
4. titanium alloy material according to claim 1, is characterized in that: in described vacuum annealing step, and described Heating temperature is 850-880 DEG C, and soaking time is 1 ~ 1.5h, and vacuum tightness is 1.0 × 10 -3~ 10 -4pa.
5. titanium alloy material according to claim 1, is characterized in that: in described electro-chemical polish step, adopts electrochemical etching to carry out aftertreatment, obtains the finished product that surfaceness is 0.6 μm ~ 0.7 μm.
6. according to the titanium alloy material described in claim 1 to 5, it is characterized in that: the tensile strength of described finished product is 800 ~ 850MPa, and unit elongation and relative reduction in area are respectively 20% and 18%.
7. according to the titanium alloy material described in claim 1 to 6, it is characterized in that: titanium alloy powder raw material packet prepared by described powder is containing following elementary composition: Al:2.80%, Zn:0.15%, Zr:0.85%, Hf:0.40%, V:2.50%, Ge:0.35%, Nd:0.70%, Nb:0.50%, Ce:1.50%, surplus is Ti.
CN201510936053.9A 2015-12-15 2015-12-15 Ce and Nd reinforced titanium alloy material Pending CN105506370A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110499438A (en) * 2019-09-30 2019-11-26 广东省航空航天装备技术研究所 Material compositions, titanium alloy product and preparation method thereof

Citations (4)

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Publication number Priority date Publication date Assignee Title
EP0202791A1 (en) * 1985-04-25 1986-11-26 Daido Tokushuko Kabushiki Kaisha Titanium alloys
CN1031721A (en) * 1987-09-01 1989-03-15 中国科学院金属研究所 A kind of heat-resistant titanium alloy
CN102120261A (en) * 2011-04-20 2011-07-13 林锦新 Method for preparing titanium product
CN104245975A (en) * 2011-11-10 2014-12-24 法国雷恩国立应用科学学院 Method for manufacturing a titanium alloy for biomedical devices

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0202791A1 (en) * 1985-04-25 1986-11-26 Daido Tokushuko Kabushiki Kaisha Titanium alloys
CN1031721A (en) * 1987-09-01 1989-03-15 中国科学院金属研究所 A kind of heat-resistant titanium alloy
CN102120261A (en) * 2011-04-20 2011-07-13 林锦新 Method for preparing titanium product
CN104245975A (en) * 2011-11-10 2014-12-24 法国雷恩国立应用科学学院 Method for manufacturing a titanium alloy for biomedical devices

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110499438A (en) * 2019-09-30 2019-11-26 广东省航空航天装备技术研究所 Material compositions, titanium alloy product and preparation method thereof

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