CN106694897B - A method of preparing tungsten Penetrator block materials - Google Patents

A method of preparing tungsten Penetrator block materials Download PDF

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Publication number
CN106694897B
CN106694897B CN201611222743.9A CN201611222743A CN106694897B CN 106694897 B CN106694897 B CN 106694897B CN 201611222743 A CN201611222743 A CN 201611222743A CN 106694897 B CN106694897 B CN 106694897B
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powder
tungsten
nano composite
mixed
iron
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CN106694897A (en
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黄伟明
尚福军
黄伟
陈子明
杨文智
张保玉
张将
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Chinese Academy of Ordnance Science Ningbo Branch
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Chinese Academy of Ordnance Science Ningbo Branch
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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
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/14Making metallic powder or suspensions thereof using physical processes using electric discharge
    • 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/045Alloys based on refractory metals
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C27/00Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04Alloys based on tungsten or molybdenum
    • 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

Abstract

A method of tungsten Penetrator block materials being prepared, step: tungsten powder, nickel powder needed for high density tungsten alloy, iron powder uniformly being mixed using high speed mixer, powder size 3um~10um;Mixed-powder powder feeder is sent into plasma powder manufacturing apparatus, gasifies in superhigh temperature plasma arc, rapidly cools to form nano composite powder, nano composite powder granularity is in 10nm~100nm;Proper amount of nano composite powder is put into graphite jig; in resistance sintering equipment; 20~40min of vacuum outgas; it is re-filled with argon gas to be protected, upper and lower stamping press is maintained at 30MPa~100MPa, electrified regulation; 1100 DEG C~1250 DEG C are warming up to the heating rate of 30~40 DEG C/min; continue to keep the temperature 1min~3min, finally be cooled to room temperature under the cooling velocity per minute greater than 50 DEG C to get required bulk material.Present invention process advantages of simple, easy to operate, the bulk material consistency of preparation is high, and plasticity is strong, has biggish application value.

Description

A method of preparing tungsten Penetrator block materials
Technical field
The present invention relates to a kind of method for preparing nano composite powder and its block materials more particularly to a kind of prepare tungsten base The method of heavy alloy nano composite powder and its block materials.
Background technique
Tungsten Penetrator has very high density, intensity, hardness and certain ductility, is widely used in aviation, boat It, military and nuclear industry.It is used as balance counterweight, damper etc. in aerospace industry;It is widely used in war industry Kinetic energy penetrator and broken first material;It is used as in nuclear industry towards plasma facing materials etc..With the hair of science and technology Exhibition, to the obdurability of tungsten alloy material, more stringent requirements are proposed, wherein refinement crystal grain is the important channel of tungsten alloy Strengthening and Toughening. Traditional tungsten alloy material is to mix micron-sized powder, carry out liquid-phase sintering again after molding or cold isostatic compaction and At.Liquid phase sintering conditions are higher (generally 1480~1600 DEG C), and sintering time is long, and the partial size of the tungsten particle of formation is larger, and one As at 30~60 μm.In recent years, domestic and international material worker was sintered using nanometer powder, the tungsten alloy crystal grain prepared It is relatively thin, reach 10 μm hereinafter, but tungsten particle is usually multilateral shape, the plasticity of material is very low, limits application.Therefore guaranteeing While densification, obtaining tiny spherical tungsten particle tissue is the Key technique problem for preparing nanometer tungsten alloy material.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of method for preparing tungsten Penetrator block materials, systems Standby simple process, easy to operate, bulk material consistency height obtained, plasticity are strong.
The technical scheme of the invention to solve the technical problem is: a kind of prepare tungsten Penetrator block material The method of material, it is characterised in that the following steps are included:
1) tungsten powder, nickel powder needed for high density tungsten alloy, iron powder are uniformly mixed using high speed mixer;
2) above-mentioned mixed mixed-powder powder feeder is sent into plasma powder manufacturing apparatus, in superhigh temperature plasma Gasify in arc, then rapidly cools to form that alloying is good, the rounded nano composite powder of appearance, nano composite powder Granularity is in 10nm~100nm;
3) proper amount of nano composite powder is put into graphite jig, in resistance sintering equipment, vacuum outgas 20~ 40min is re-filled with argon gas and is protected, and upper and lower stamping press is maintained at 30MPa~100MPa, electrified regulation, with 30~40 DEG C/ The heating rate of min is warming up to 1100 DEG C~1250 DEG C, continues to keep the temperature 1min~3min, finally cold greater than 50 DEG C per minute But it is cooled to room temperature under speed to get required bulk material;
Powder in the step 1 is made of following raw material as unit of weight: 91-97 parts of tungsten powder, nickel powder 6.3-2.1 Part, 2.7-0.9 parts of iron powder;
The raw material tungsten powder, nickel powder, iron powder granularity be 3-10um;
As an improvement, the incorporation time of tungsten powder, nickel powder, iron powder in the step 1) is 9~11h.
As an improvement, the mixing of the powder in the step 1), storage and transportational process are protected in vacuum or inert gas Shield is lower to be carried out.
It improves again, the air pressure that mixed-powder gasifies in superhigh temperature plasma arc in the step 2) is 1.0 × 105Pa- 1.2×105Pa, temperature are 10000-12000 DEG C.
Finally, the vacuum outgas 30min in the step 3), heating rate is 35 DEG C/min.
Compared with the prior art, the advantages of the present invention are as follows: selection plasma powder manufacturing apparatus, micron-sized alloy powder It is gasified totally, evaporates metal gas atom, be quickly cooled down in an inert atmosphere, forming core is deposited near plasma arcs, and Grow into spherical nano composite powder;Nanometer powder is powered pressure sintering in graphite jig, on the surface of pulse current Activation and ball shaped nano powder itself under accumulation densification, can quick densifying, be lower than liquid phase sintering conditions Under fine and close block materials are obtained with very short time.Present invention process advantages of simple, easy to operate, the bulk material cause of preparation Density is high, and plasticity is strong, has biggish application value, can be used conveniently to prepare ball shaped nano alloy powder and block nanometer material Material.
Detailed description of the invention
Fig. 1 is nano composite powder shape appearance figure prepared by the present invention;
Fig. 2 is the metallographic structure figure that alloy is made of electric discharge pressure sintering by the present invention.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1
The powder such as appropriate tungsten powder, nickel powder, iron powder needed for heavy alloy are weighed, are uniformly mixed in high speed mixer 9h, mixing, storage and the transportational process of powder carry out under vacuum or inert gas shielding;
The powder is made of following raw material as unit of weight: 91 parts of tungsten powder, 6.3 parts of nickel powder, 2.7 parts of iron powder;
The raw material tungsten powder, nickel powder, iron powder granularity be 3-4um;
Mixed-powder powder feeder is sent into plasma powder manufacturing apparatus, is gasified in superhigh temperature plasma arc, air pressure It is 1.0 × 105Pa, temperature are 10000 DEG C, rapidly cool to form that alloying is good, the rounded nano composite powder of appearance, The granularity of nano composite powder is in 10nm~30nm, and the shape appearance figure of nano composite powder made from the present embodiment is as shown in Figure 1, can To see that appearance is spherical in shape;
Proper amount of nano composite powder is put into graphite jig, in resistance sintering equipment, vacuum outgas 30min, then fill Enter argon gas to be protected, upper and lower stamping press is maintained at 30MPa, and electrified regulation is warming up to 1100 with the heating rate of 30 DEG C/min DEG C, continue to keep the temperature 1min, finally be cooled to room temperature under the cooling velocity per minute greater than 50 DEG C to get required block-shaped material Expect, the metallographic structure figure of alloy made from the present embodiment is as shown in Figure 2, it can be seen that forms fine and compact block structure.
Embodiment 2
The powder such as appropriate tungsten powder, nickel powder, iron powder needed for heavy alloy are weighed, are uniformly mixed in high speed mixer 10h, the granularity of powder are chosen at 5um~7um, and mixing, storage and the transportational process of powder are in vacuum or inert gas shielding Lower progress;
The powder is made of following raw material as unit of weight: 93 parts of tungsten powder, 4.9 parts of nickel powder, 2.1 parts of iron powder;
The raw material tungsten powder, nickel powder, iron powder granularity be 5-7um;
Mixed-powder powder feeder is sent into plasma powder manufacturing apparatus, is gasified in superhigh temperature plasma arc, air pressure It is 1.1 × 105Pa, rapidly cools to form that alloying is good by 11000 DEG C of temperature, and the rounded nano composite powder of appearance is received The granularity of rice composite powder is in 30nm~70nm;
Proper amount of nano composite powder is put into graphite jig, in resistance sintering equipment, vacuum outgas 30min, then fill Enter argon gas to be protected, upper and lower stamping press is maintained at 70MPa, and electrified regulation is warming up to 1150 with the heating rate of 35 DEG C/min DEG C, continue to keep the temperature 2min, finally be cooled to room temperature under the cooling velocity per minute greater than 50 DEG C to get required block-shaped material Material.
Embodiment 3
The powder such as appropriate tungsten powder, nickel powder, iron powder needed for heavy alloy are weighed, are uniformly mixed in high speed mixer 11h, the granularity of powder are chosen at 8um~10um, and mixing, storage and the transportational process of powder are in vacuum or inert gas shielding Lower progress;
The powder is made of following raw material as unit of weight: 97 parts of tungsten powder, 2.1 parts of nickel powder, 0.9 part of iron powder;
The raw material tungsten powder, nickel powder, iron powder granularity be 8-10um;
Mixed-powder powder feeder is sent into plasma powder manufacturing apparatus, is gasified in superhigh temperature plasma arc, air pressure It is 1.2 × 105Pa, rapidly cools to form that alloying is good by 12000 DEG C of temperature, and the rounded nano composite powder of appearance is received The granularity of rice composite powder is in 70nm~100nm;
Proper amount of nano composite powder is put into graphite jig, in resistance sintering equipment, vacuum outgas 40min, then fill Enter argon gas to be protected, upper and lower stamping press is maintained at 100MPa, and electrified regulation is warming up to 1250 with the heating rate of 40 DEG C/min DEG C, continue to keep the temperature 3min, finally be cooled to room temperature under the cooling velocity per minute greater than 50 DEG C to get required block-shaped material Material.
Following table lists 1-3 of embodiment of the present invention heavy alloy and conventional liquid phase sintering high-density alloy in relative density And the comparison in plasticity, as a result as shown in the table.
The test result carries out after conventional stress relief annealing process in alloy, and relative density is surveyed using drainage Examination makees percentage with theoretical density, and plasticity is indicated using the elongation percentage in tensile strength test.
It can be seen from table after applying the present invention, the relative density and plasticity of alloy are all improved.

Claims (5)

1. a method of prepare tungsten Penetrator block materials, it is characterised in that the following steps are included:
1) tungsten powder, nickel powder needed for high density tungsten alloy, iron powder are uniformly mixed using high speed mixer;
2) above-mentioned mixed mixed-powder powder feeder is sent into plasma powder manufacturing apparatus, in superhigh temperature plasma arc Gasification, then rapidly cools to form that alloying is good, the rounded nano composite powder of appearance, the granularity of nano composite powder In 10nm~100nm;
3) proper amount of nano composite powder is put into graphite jig, in resistance sintering equipment, 20~40min of vacuum outgas, then It is filled with argon gas to be protected, upper and lower stamping press is maintained at 30MPa~100MPa, electrified regulation, with the heating of 30~40 DEG C/min Speed is warming up to 1100 DEG C~1250 DEG C, continues to keep the temperature 1min~3min, finally under the cooling velocity per minute greater than 50 DEG C It is cooled to room temperature to get required bulk material;
Powder in the step 1 is made of following raw material as unit of weight: 91-97 parts of tungsten powder, 6.3-2.1 parts of nickel powder, iron 2.7-0.9 parts of powder;
The raw material tungsten powder, nickel powder, iron powder granularity be 3-10um.
2. according to the method described in claim 1, it is characterized by: when the mixing of tungsten powder, nickel powder, iron powder in the step 1) Between be 9~11h.
3. according to the method described in claim 1, it is characterized by: the mixing of the powder in the step 1), storage and transport Process carries out under vacuum or inert gas shielding.
4. according to the method described in claim 1, it is characterized by: mixed-powder is in superhigh temperature plasma arc in the step 2) The air pressure of middle gasification is 1.0 × 105Pa-1.2×105Pa, temperature are 10000-12000 DEG C.
5. according to the method described in claim 1, it is characterized by: vacuum outgas 30min in the step 3), heating rate For 35 DEG C/min.
CN201611222743.9A 2016-12-27 2016-12-27 A method of preparing tungsten Penetrator block materials Active CN106694897B (en)

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CN107630161A (en) * 2017-07-26 2018-01-26 宜兴新高合金制品有限公司 A kind of motor for cell phone mass preparation method and its manufacturing system
CN111283212B (en) * 2020-03-27 2022-05-17 陕西理工大学 Tungsten alloy material with stripping self-sharpening structure and preparation method and application thereof

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CN101245431A (en) * 2008-03-25 2008-08-20 长春工业大学 Gamma-group Ti-Al alloy material with high-temperature resistance oxidation and manufacture method thereof
CN101269834B (en) * 2008-05-19 2011-04-06 昆明理工大学 Method for producing nano-ITO powder with plasma electrical arc one-step method
JP5094668B2 (en) * 2008-09-30 2012-12-12 株式会社日清製粉グループ本社 Method for producing Ni-W alloy fine particles and method for producing Ni-W alloy fine particles
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CN104525943A (en) * 2014-11-21 2015-04-22 长安大学 Pressurizing device for preparing high-density ultrafine grain tungsten block and application of pressurizing device
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