CN110524001A - A kind of preparation method of peritectoid titanium alloy powder - Google Patents
A kind of preparation method of peritectoid titanium alloy powder Download PDFInfo
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- CN110524001A CN110524001A CN201910977208.1A CN201910977208A CN110524001A CN 110524001 A CN110524001 A CN 110524001A CN 201910977208 A CN201910977208 A CN 201910977208A CN 110524001 A CN110524001 A CN 110524001A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/10—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE 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
- B33Y70/00—Materials specially adapted for additive manufacturing
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C14/00—Alloys based on titanium
Abstract
The invention discloses a kind of preparation methods of peritectoid titanium alloy powder: CP titanium powder and TC4 alloy powder are used straight argon gas washing in a vacuum respectively；By CP titanium powder as described below, La and the TC4 alloy powder, investment vacuum sintering furnace carries out the obtained alloy bar of melting in order respectively again, and the alloy bar is finally obtained spherical powder using rotating electrode atomized method.Powder hollow rate produced by the present invention is low, good fluidity, is suitable for 3D printing.
Description
Technical field
The invention belongs to 3D printing material manufacturing fields, in particular to a kind of preparation side of peritectoid titanium alloy powder
Method.
Background technique
3D printing technique is also known as increasing material manufacturing, is that one kind does not need machining or mold can be soft in conjunction with computer
Data in part strafe liquid, powder or sheeting, are successively superimposed as the advanced technology of the product of any shape.It is greatly
The lead time for shortening product, production efficiency is improved, is particularly suitable for that structure is complicated, extensive manufacture, customization of individual character
Product, great exploitation potential.The core of 3D printing is equipment and material.The material category used that matches at present with equipment is few,
Performance is unstable, becomes the bottleneck problem for restricting 3D printing technique application and development.
Titanium is a kind of important structural metal, and titanium alloy intensity is high, and high temperature resistant, density is small, can be widely used for military project, changes
The fields such as work, biomedicine, but since the chemical activity of titanium is big, violent strong reaction can occur with O, H, N, it is raw
It is big to produce difficulty.In addition to adapting to the 3D printing technique based on powder, good fluidity is prepared, oxygen content is low, and sphericity is high, powder
The last uniform titanium alloy powder of particle size distribution, has also been proposed higher requirement to production technology.
Currently, preparation is suitable for 3D printing technique titanium alloy powder, atomization is mostly used, principle is to be swashed to fall with fluid
Molten metal is condensed into rapidly powder particle at droplet.It is limited by material and facility, mostly nebulization efficiency is relatively low, system
Standby the rate of production of fine powder is not also high.In addition atomization is most of blows off metallic particles by inert gas, is easy village hollowing.In product ball
During shape, the too small nano particle of a large amount of partial size is generated, compromises the overall flow of product, and target product yield
It is too low.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides a kind of preparation method of peritectoid titanium alloy powder, use is dilute
There is metal La peritectoid CP titanium powder to form a kind of peritectic structure, then crystal phase circle is diffused into TC4, plasma rotating electrode process system
Standby powder chemistry ingredient is approximate with material composition, and good sphericity, and without hollow, particle is smooth, and powder flowbility is good, meets 3D
Requirement of the printing technique to powder.
In order to reach the goals above, the invention adopts the following technical scheme:
A kind of preparation method of peritectoid titanium alloy powder, which comprises the steps of:
S1, CP titanium powder and TC4 alloy powder are used into straight argon gas washing in a vacuum respectively；
S2, by following CP titanium powder, La and TC4 alloy powder, investment vacuum sintering furnace carries out the obtained alloy of melting in order respectively
Stick, three kinds of Parts by Ingredients are respectively 20-60 parts of CP titanium, 1-5.5 parts of LA, 30-50 parts of TC4；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method.
Preferably, the impurity mass percent in CP titanium powder are as follows: Fe≤0.3%, C≤0.08%, N≤0.05%, H≤
0.015%, O≤0.25%.
Preferably, each ingredient percent Al:5.5%-6.0% in TC4 powder, V:3.5%-4.5%, other impurities≤
0.01%, surplus Ti.
Preferably, three kinds of Parts by Ingredients in S2: 20-50 parts of CP titanium, 1-5.5 parts of LA, 30-50 parts of TC4.
Preferably, CP titanium powder is placed in vacuum sintering furnace in S2, is filled with inertia mobility atmosphere, then heats to 950 DEG C
~1000 DEG C, heat preservation at least 20min carries out microwave melting, puts into the La and is uniformly mixed, keeps the temperature at least 20min, be cooled to
890-900 DEG C, TC4 alloy powder is added, keeps the temperature at least 60min, is cooled to alloy bar in grinding tool, the diameter is 40~
60mm, length are 500~800mm.
Preferably, rotating electrode atomized the following steps are included:
1) it, is placed in alloy bar as consutrode in atomization plant, is filled with inertia after evacuating to atomization plant powder room
Protective gas；
2) rotation atomization, is carried out to alloy bar using atomization plant, the conjunction of peritectoid titanium can be obtained in the drop natural cooling after atomization
Bronze end.
Preparation method according to claim 6, it is characterised in that the inert protective gas being filled be helium and argon gas,
Its volume ratio is 0-2:6-8.
The present invention compared with prior art the utility model has the advantages that
A kind of peritectic structure is formed with rare metal La peritectoid CP titanium powder, then crystal phase circle is diffused into TC4, the vanadium in TC4
It is β phase, aluminium can also form peritectoid state, ultimately form approximate β phase peritectoid titanium alloy, the powder of plasma rotating electrode process preparation
Chemical component is approximate with material composition, and low village hollowing, surface is smooth, good fluidity, is suitble to 3D printing.CP titanium and TC4 facilitate easy
, cheap, the present invention is suitble to industrial application.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff every other embodiment obtained without making creative work belongs to what the present invention protected
Range.
Embodiment 1
A kind of preparation method of peritectoid titanium alloy powder, includes the following steps:
S1, by industrially pure titanium TA1 powder and TC4 alloy powder (each composition quality score are as follows: Al:6.0%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,60 parts by weight of TA1 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
980 DEG C, heat preservation 30min carries out microwave melting, and investment La5.5 parts by weight are uniformly mixed, keep the temperature 30min, be cooled to 890 DEG C, add
Enter 30 parts by weight of TC4 alloy powder, keeps the temperature 60min, alloy bar, diameter 60mm, length 500mm are cooled in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with the inertia helium and argon that volume ratio is 2:6；
2) rotation atomization, is carried out to alloy bar using atomization plant, the conjunction of peritectoid titanium can be obtained in the drop natural cooling after atomization
Bronze end.
Embodiment 2
A kind of preparation method of peritectoid titanium alloy powder, includes the following steps:
S1, by industrial pure titanium TA2 powder and TC4 alloy powder (each composition quality score are as follows: Al:6.0%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,40 parts by weight of TA2 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
980 DEG C, heat preservation 30min carries out microwave melting, and investment La4 parts by weight are uniformly mixed, and keeps the temperature 30min, is cooled to 890 DEG C, is added
40 parts by weight of TC4 alloy powder keep the temperature 60min, alloy bar, diameter 60mm, length 500mm are cooled in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with the inertia helium and argon gas that volume ratio is 2:8.
2) rotation atomization, is carried out to alloy bar using atomization plant, peritectoid can be obtained in the drop natural cooling after atomization
Titanium alloy powder.
Embodiment 3
A kind of preparation method of peritectoid titanium alloy powder, includes the following steps:
S1, by industrially pure titanium TA3 powder and TC4 alloy powder (each composition quality score are as follows: Al:6.0%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,20 parts by weight of TA3 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
980 DEG C, heat preservation 30min carries out microwave melting, and investment La1 parts by weight are uniformly mixed, and keeps the temperature 30min, is cooled to 890 DEG C, is added
50 parts by weight of TC4 alloy powder keep the temperature 60min, alloy bar, diameter 60mm, length 500mm are cooled in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with inert argon.
2) rotation atomization, is carried out to alloy bar using atomization plant, peritectoid can be obtained in the drop natural cooling after atomization
Titanium alloy powder.
Embodiment 4
A kind of preparation method of peritectoid titanium alloy powder, includes the following steps:
S1, by industrially pure titanium TA1 powder and TC4 alloy powder (each composition quality score are as follows: Al:5.5%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,40 parts by weight of TA1 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
1000 DEG C, heat preservation 30min carries out microwave melting, and investment La4 parts by weight are uniformly mixed, and keeps the temperature 30min, is cooled to 890 DEG C, is added
40 parts by weight of TC4 alloy powder keep the temperature 60min, alloy bar, diameter 40mm, length 800mm are cooled in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with inert argon；
2) rotation atomization, is carried out to alloy bar using atomization plant, the conjunction of peritectoid titanium can be obtained in the drop natural cooling after atomization
Bronze end.
Embodiment 5
A kind of preparation method of peritectoid titanium alloy powder, includes the following steps:
S1, by industrial pure titanium TA2 powder and TC4 alloy powder (each composition quality score are as follows: Al:5.5%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,40 parts by weight of TA2 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
1000 DEG C, heat preservation 30min carries out microwave melting, and investment La4 parts by weight are uniformly mixed, and keeps the temperature 30min, is cooled to 890 DEG C, is added
40 parts by weight of TC4 alloy powder keep the temperature 60min, alloy bar, diameter 40mm, length 800mm are cooled in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with inert argon；
2) rotation atomization, is carried out to alloy bar using atomization plant, the conjunction of peritectoid titanium can be obtained in the drop natural cooling after atomization
Bronze end.
Embodiment 6
A kind of preparation method of peritectoid titanium alloy powder, includes the following steps:
S1, by industrially pure titanium TA3 powder and TC4 alloy powder (each composition quality score are as follows: Al:5.5%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,40 parts by weight of TA3 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
1000 DEG C, heat preservation 30min carries out microwave melting, and investment La4 parts by weight are uniformly mixed, and keeps the temperature 30min, is cooled to 890 DEG C, is added
40 parts by weight of TC4 alloy powder keep the temperature 60min, alloy bar, diameter 40mm, length 800mm are cooled in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with inert argon；
2) rotation atomization, is carried out to alloy bar using atomization plant, the conjunction of peritectoid titanium can be obtained in the drop natural cooling after atomization
Bronze end.
Comparative example 1
A kind of preparation method of titanium alloy powder, includes the following steps:
S1, by industrially pure titanium TA1 powder and TC4 alloy powder (each composition quality score are as follows: Al:5.5%, V:4.5%, other
Impurity≤0.01%, surplus Ti) use straight argon gas washing in a vacuum respectively；
S2,40 parts by weight of TA1 powder and 40 parts by weight of TC4 alloy powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa fills
Enter inert argon, then heat to 1000 DEG C, keep the temperature 60min, carries out melting and be cooled to alloy bar in grinding tool, diameter is
40mm, length 800mm；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with inert argon；
2) rotation atomization, is carried out to alloy bar using atomization plant, Titanium Powder can be obtained in the drop natural cooling after atomization
End.
Comparative example 2
S1, industrially pure titanium TA1 powder is used into straight argon gas washing in a vacuum respectively；
S2,40 parts by weight of TA1 powder are placed in vacuum sintering furnace, vacuum degree 10-3Pa is filled with inert argon, then heats to
1000 DEG C, 60min is kept the temperature, melting is carried out and is cooled to alloy bar, diameter 40mm, length 800mm in grinding tool；
S3, alloy bar is obtained into spherical powder using rotating electrode atomized method:
1) it, is placed in alloy bar as consutrode in atomization plant, atomization plant powder room is carried out being evacuated to vacuum degree
It is 10-3Pa is filled with inert argon；
2) rotation atomization, is carried out to alloy bar using atomization plant, Titanium Powder can be obtained in the drop natural cooling after atomization
End.
It is to above embodiments progress quantitative measurement and result is tabulated below:
The peritectoid titanium alloy powder prepared by the method for the invention as seen from the above table has good mobility, and excellent pine fills close
Degree, most of hollow rate≤3%, hollow rate is low, and LA content is lower in embodiment 3, it may be possible to because to the earlier packet of CP titanium powder
Brilliant degree is low, and intracrystalline diffusion degree of the later period in TC4 is inadequate, causes to generate undesirable hollow rate and powder flowbility.On
It states powder obtained in embodiment and is suitable for 3D powder printing engineering.
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this
The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, and the present invention is not limited to above-mentioned implementations
, equivalent change or modification made by all Spirit Essences according to the present invention should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of peritectoid titanium alloy powder, which comprises the steps of:
S1, CP titanium powder and TC4 alloy powder are used into straight argon gas washing in a vacuum respectively；
S2, by CP titanium powder as described below, La and the TC4 alloy powder, investment vacuum sintering furnace carries out melting in order respectively
Alloy bar is made, three kinds of Parts by Ingredients are respectively 20-60 parts of CP titanium, 1-5.5 parts of LA, 30-50 parts of TC4；
S3, the alloy bar is obtained into spherical powder using rotating electrode atomized method.
2. preparation method according to claim 1, which is characterized in that the impurity mass percent in the CP titanium powder
Are as follows: Fe≤0.3%, C≤0.08%, N≤0.05%, H≤0.015%, O≤0.25%.
3. preparation method according to claim 1, which is characterized in that each ingredient percent Al in the TC4 powder:
5.5%-6.0%, V:3.5%-4.5%, other impurities≤0.01%, surplus Ti.
4. preparation method according to claim 1, which is characterized in that three kinds of Parts by Ingredients in the S2: CP titanium 20-50
Part, 1-5.5 parts of LA, 30-50 parts of TC4.
5. preparation method according to claim 1-4, which is characterized in that CP titanium powder described in S2 is placed in vacuum and burns
Freezing of a furnace is filled with inertia mobility atmosphere, then heats to 950 DEG C~1000 DEG C, and heat preservation at least 20min carries out microwave melting, throws
Enter the La to be uniformly mixed, keep the temperature at least 20min, be cooled to 890-900 DEG C, TC4 alloy powder is added, keeps the temperature at least 60min,
Alloy bar is cooled in grinding tool, the diameter is 40~60mm, and length is 500~800mm.
6. preparation method according to claim 5, which is characterized in that it is rotating electrode atomized the following steps are included:
1) it, is placed in alloy bar as consutrode in atomization plant, is filled with inertia after evacuating to atomization plant powder room
Protective gas；
2) rotation atomization, is carried out to alloy bar using atomization plant, the conjunction of peritectoid titanium can be obtained in the drop natural cooling after atomization
Bronze end.
7. preparation method according to claim 6, it is characterised in that the inert protective gas being filled be helium and argon gas,
Volume ratio is 0-2:6-8.
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| CN201910977208.1A CN110524001A (en) | 2019-10-15 | 2019-10-15 | A kind of preparation method of peritectoid titanium alloy powder |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114178538A (en) * | 2021-11-19 | 2022-03-15 | 西南交通大学 | Preparation method of ultrahigh-sphericity nanometer yttrium oxide dispersion-strengthened titanium alloy powder |
-
2019
- 2019-10-15 CN CN201910977208.1A patent/CN110524001A/en not_active Withdrawn
Non-Patent Citations (1)
| Title |
|---|
| 唐代明: "《金属材料学》", 30 June 2014, 西南交通大学出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114178538A (en) * | 2021-11-19 | 2022-03-15 | 西南交通大学 | Preparation method of ultrahigh-sphericity nanometer yttrium oxide dispersion-strengthened titanium alloy powder |
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Application publication date: 20191203 |