CN110052616A - A kind of 3D printing alloy powder and preparation method thereof - Google Patents
A kind of 3D printing alloy powder and preparation method thereof Download PDFInfo
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- CN110052616A CN110052616A CN201910477507.9A CN201910477507A CN110052616A CN 110052616 A CN110052616 A CN 110052616A CN 201910477507 A CN201910477507 A CN 201910477507A CN 110052616 A CN110052616 A CN 110052616A
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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
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
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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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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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
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
- C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
- C22C29/08—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds based on tungsten carbide
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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
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The present invention relates to 3D printing technique fields, more particularly to a kind of 3D printing alloy powder and preparation method thereof, preparation method provided by the invention, comprising the following steps: ball milling after mixing graphene, tungsten carbide powder, cobalt powder and carbonization chromium powder obtains mixed metal powder；The mixed metal powder is subjected to induction plasma spheroidising, obtains 3D printing alloy powder.Use graphene for carbon source in the preparation method provided by the invention, wherein graphene is with sp2Hybridized orbit is in the single layer two dimensional crystal that honeycomb lattice is arranged to make up, and each carbon atom is connected by very strong σ key with other 3 carbon atoms, these strong carbon-carbon bonds cause graphene sheet layer to have excellent mechanical property and structural rigidity.The graphene of ultra-thin two-dimension lamellar structure has very high chemical activity and biggish specific surface area simultaneously, improves reaction rate, reduces reaction temperature, while shortening the manufacturing cycle of product.
Description
Technical field
The present invention relates to 3D printing technique fields more particularly to a kind of 3D printing alloy powder and preparation method thereof.
Background technique
3D printing is a kind of increases material manufacturing technology that three dimensional articles are obtained by layer-by-layer added material.Usually seen 3D is beaten
Print material has filiform, powdered metal, plastics, ceramics etc..Although 3D printing technique obtains hair at full speed in recent years
Exhibition, but the research and development in terms of material are relatively slow, limit the extensive use of 3D printing technique.
The preparation process reaction temperature of 3D printing alloy powder is higher in the prior art, long preparation period, therefore, how
3D printing alloy powder is prepared in lower reaction temperature, shorter time, there are no preferred solutions in the prior art.
Summary of the invention
The purpose of the present invention is to provide a kind of 3D printing alloy powder and preparation method thereof, the preparation method reaction speed
Rate is high, and reaction temperature is low, short preparation period.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of preparation methods of 3D printing alloy powder, comprising the following steps:
Ball milling after graphene, tungsten carbide powder, cobalt powder and carbonization chromium powder are mixed, obtains mixed metal powder；
The mixed metal powder is subjected to induction plasma spheroidising, obtains 3D printing alloy powder.
Preferably, the mass ratio of the graphene, tungsten carbide powder, cobalt powder and the chromium powder that is carbonized is (5.5~6.5): (80~
95): (5~15): (0.2~0.5).
Preferably, the ball milling is wet ball grinding；
The revolving speed of the wet ball grinding is 30~36r/min, and the time of the wet ball grinding is 24~36 hours.
Preferably, the partial size of the mixed metal powder is 200~300 mesh.
Preferably, after the ball milling further include: the powder after the ball milling is sieved and dried, mixed metal is obtained
Powder；The temperature of the drying is 90~95 DEG C, and the time of the drying is 2.5~4h.
Preferably, the ion-gas gas source of the induction plasma spheroidising is Ar and H2, the Ar and H2Volume be than
(22~26): 1.
Preferably, the power of the induction plasma spheroidising is 45~60kW.
Preferably, the powder feeding rate of the induction plasma spheroidising is 5~10kg/h.
The present invention also provides the 3D printing alloy powder that the preparation method is prepared, the 3D printing alloy powder
Partial size be 45~105 μm.
The present invention provides a kind of preparation methods of 3D printing alloy powder, comprising the following steps: by graphene, tungsten carbide
Ball milling after powder, cobalt powder and carbonization chromium powder mixing, obtains mixed metal powder；The mixed metal powder is subjected to induction plasma
Spheroidising obtains 3D printing alloy powder.Use graphene for carbon source in the preparation method provided by the invention, wherein stone
Black alkene is with sp2Hybridized orbit is in the single layer two dimensional crystal that is arranged to make up of honeycomb lattice, each carbon atom by very strong σ key with
Other 3 carbon atoms are connected, these strong carbon-carbon bonds cause graphene sheet layer to have excellent mechanical property and structure rigid
Property.The graphene of ultra-thin two-dimension lamellar structure has very high chemical activity and biggish specific surface area simultaneously, improves anti-
Rate is answered, reaction temperature is reduced, shortens the manufacturing cycle of product；Induction plasma spheroidising simultaneously can effectively change
The physics and chemical characteristic of kind powder, being mainly manifested in improves the mobility of alloy powder, the porosity for reducing powder, improves powder
Last density, improves particle surface finish, improves powder purity, is precisely controlled oxygen content the brittleness for reducing powder.
Detailed description of the invention
Fig. 1 is the HRTEM figure for the 3D printing alloy powder that embodiment 1 is prepared；
Fig. 2 is the SEM figure for the 3D printing alloy powder that embodiment 1 is prepared.
Specific embodiment
The present invention provides a kind of preparation methods of 3D printing alloy powder, comprising the following steps:
Ball milling after graphene, tungsten carbide powder, cobalt powder and carbonization chromium powder are mixed, obtains mixed metal powder；
The mixed metal powder is subjected to induction plasma spheroidising, obtains 3D printing alloy powder.
In the present invention, if without specified otherwise, all raw material components are commercial product well known to those skilled in the art.
Ball milling after the present invention mixes graphene, tungsten carbide powder, cobalt powder and carbonization chromium powder, obtains mixed metal powder；?
In the present invention, the graphene, tungsten carbide powder, cobalt powder and be carbonized chromium powder partial size it is independent preferably 10~15 μm, more preferably
It is 11~14 μm, most preferably 12~13 μm.In the present invention, the partial size is preferably Fisher particle size.
In the present invention, the graphene, tungsten carbide powder, cobalt powder and be carbonized chromium powder mass ratio be preferably (5.5~
6.5): (80~95): (5~15): (0.2~0.5), more preferably (5.8~6.2): (85~92): (8~12): (0.24~
0.4), most preferably (5.9~6.13): (88~90): (9~10): (0.3~0.32).In the present invention, the mass ratio is excellent
Choosing is based on it can obtain WC-8Co hard alloy.
In the present invention, the graphene, tungsten carbide powder and cobalt powder are reaction raw materials；The carbonization chromium powder is fining agent,
Play the role of refining crystal grain.
In the present invention, the ball milling is preferably wet ball grinding；The ball-milling medium of the wet ball grinding is preferably ethyl alcohol.?
In the present invention, the graphene, tungsten carbide powder, cobalt powder and be carbonized chromium powder gross mass and ethyl alcohol mass ratio be preferably (8~
10): (2~3), more preferably (8.5~9.5): (2.2~2.8), most preferably (8.8~9.2): (2.4~2.6).
In the present invention, the revolving speed of the wet ball grinding is preferably 30~36r/min, more preferably 31~35r/min, most
Preferably 32~34r/min；The time of the wet ball grinding is preferably 24~36 hours, more preferably 26~34 hours, optimal
It is selected as 28~32 hours.
In the present invention, after the ball milling it is also preferable to include: the powder after the ball milling is sieved and is dried, is obtained
Mixed metal powder；The present invention is to the no any special restriction of screening, using screening well known to those skilled in the art
Process is sieved and obtains the powder that partial size is 200~300 mesh.
In the present invention, the temperature of the drying is preferably 90~95 DEG C, and more preferably 91~94 DEG C, most preferably 92~
93℃；The time of the drying is preferably 2.5~4h, more preferably 2.8~3.8h, most preferably 3.2~3.6h.In the present invention
In, the drying is preferably dried in vacuo.
In the present invention, the partial size of the mixed metal powder is preferably 200~300 mesh, more preferably 220~280 mesh,
Most preferably 240~260 mesh.
It is last to obtain mixed metal powder, the mixed metal powder is carried out induction plasma spheroidising by the present invention, is obtained
To 3D printing alloy powder.
In the present invention, the ion-gas gas source of the induction plasma spheroidising is preferably Ar and H2, the Ar and H2's
Volume ratio is preferably (22~26): 1, more preferable (23~25): 1, most preferably (23.5~24.5): 1；The induction plasma
The quenching gas of spheroidising is preferably the Ar recycled.In the present invention, the power of the induction plasma spheroidising is preferred
For 45~60kW, more preferably 46~49Kw, most preferably 47~48Kw.In the present invention, at the induction plasma nodularization
The powder feeding rate of reason is preferably 5~10Kg/h, more preferably 6~9Kg/h, most preferably 7~8Kg/h.
After the completion of induction plasma spheroidising, the present invention is preferably received from the reactor bottom of induction plasma spheroidising
Collect mixture, and sieved, obtains 3D printing alloy powder.
The present invention to the no any special restriction of the screening, using screening process well known to those skilled in the art into
Row sieves and obtains the 3D printing alloy powder that partial size is 45~105 μm.
The present invention also provides the 3D printing alloy powder that the preparation method is prepared, the 3D printing alloy powder
Partial size be preferably 45~105 μm, more preferably 60~80 μm, most preferably 65~75 μm.In the present invention, the 3D printing
The structure of alloy powder is ball-type.
3D printing alloy powder provided by the invention is described in detail below with reference to embodiment, but cannot be it
Be interpreted as limiting the scope of the present invention.
Embodiment 1
It is the graphene of 10~15 μm of 5.9kg, the tungsten carbide powder of 92kg, the cobalt powder of 8kg, the carbon of 0.4kg by partial size
The ethyl alcohol for changing chromium powder and 31.89L is mixed and is carried out wet ball grinding 32 hours under the revolving speed of 30r/min, 270 mesh sieving, 90
It is dried in vacuo 2.5 hours under conditions of DEG C, obtains mixed metal powder；
Using Ar and H2Ar for plasma source (volume ratio 24:1), circulation is quenching gas, and power 45kW is sent
Powder rate is the condition of 5kg/h, carries out induction plasma spheroidising to the mixed metal powder, is collected from reactor bottom mixed
Material is closed, screening obtains the 3D printing alloy powder that partial size is 45~105 μm；
Fig. 1 is the HRTEM figure of 3D printing alloy powder obtained by the present embodiment, and the upper left corner Fig. 1 is the transmission of interface high-resolution
Electronic Speculum enlarged drawing, image show, graphene has extraordinary flexibility, by foring and WC in the distortion of interface atom
The higher matching of atom in crystal grain, WC grain atom does not strain substantially, and atomic arrangement has occurred largely in graphene
Bending and deformation, but still maintain the ordered arrangement of atom.It is answered it can be seen that graphene can play to improve to absorb in alloy
The effect of power.Graphene is not broken by self-deformation, on the one hand can offset extraneous work done, on the other hand can be very
Good ground resistance stops the extension of dislocation crack, protects the integrality of WC grain, and collaboration Binder Phase improves intensity and the increasing of alloy jointly
Its strong greasy property；
Fig. 2 is that the SEM of the 3D printing alloy powder schemes, and as seen from the figure, 3D printing alloy powder of the present invention is
Ball shape structure.
Embodiment 2
It is the tungsten carbide powder of the graphene 46kg of 10~15 μm of 2.95kg, the cobalt powder of 4kg, the carbon of 0.2kg by partial size
The ethyl alcohol for changing chromium powder and 15.945L is mixed and is carried out wet ball grinding 30 hours under the revolving speed of 32r/min, 270 mesh sieving, 90
It is dried in vacuo 2.5 hours under conditions of DEG C, obtains mixed metal powder；
Using Ar and H2Ar for plasma source (volume ratio 25:1), circulation is quenching gas, and power 46kW is sent
Powder rate is the condition of 6kg/h, carries out induction plasma spheroidising to the mixed metal powder, is collected from reactor bottom mixed
Material is closed, screening obtains the 3D printing alloy powder that partial size is 45~105 μm.
Embodiment 3
It is the graphene of 10~15 μm of 11.8kg by partial size, the tungsten carbide powder of 184kg, the cobalt powder of 16kg, 0.8kg's
The ethyl alcohol of carbonization chromium powder and 63.78L are mixed and are carried out wet ball grinding 34 hours under the revolving speed of 36r/min, the sieving of 270 mesh,
It is dried in vacuo 2.5 hours under conditions of 90 DEG C, obtains mixed metal powder；
Using Ar and H2Ar for plasma source (volume ratio 26:1), circulation is quenching gas, and power 48kW is sent
Powder rate is the condition of 7kg/h, carries out induction plasma spheroidising to the mixed metal powder, is collected from reactor bottom mixed
Material is closed, screening obtains the 3D printing alloy powder that partial size is 45~105 μm.
Embodiment 4
According to GB1482-84 standard, the 3D printing alloy powder that Examples 1 to 3 is obtained carries out flow velocity test, according to
GB1479-84 standard, the 3D printing alloy powder that Examples 1 to 3 is obtained carries out the test of apparent density, according to GB4164-
84 standards, the 3D printing alloy powder that Examples 1 to 3 is obtained carry out the test of oxygen content, and test result is as shown in table 1:
The physical property for the 3D printing alloy powder that 1 Examples 1 to 3 of table obtains
| Embodiment | Flow velocity (S/50g) | Apparent density (g/cm3) | Oxygen content (%) |
| Embodiment 1 | 13.3 | 5.25 | 0.016 |
| Embodiment 2 | 15.1 | 5.46 | 0.018 |
| Embodiment 3 | 14.6 | 5.32 | 0.016 |
As shown in Table 1, have using the 3D printing alloy powder that preparation method of the present invention is prepared preferable
Mobility (flow velocity is 13.3~15.1S/50g), powder density (5.25~5.46g/cm3) be also improved, while can
Oxygen content is accurately controlled below 0.018%.
The 3D printing alloy powder that Examples 1 to 3 is obtained carries out screening test, and test result is as shown in table 2:
The size distribution for the 3D printing alloy powder that 2 Examples 1 to 3 of table obtains
| Embodiment | (-43+53)μm | (-53+75)μm | (-75+90)μm | (-90+105)μm |
| Embodiment 1 | 18.4% | 54.6% | 14.9% | 12.1% |
| Embodiment 2 | 22.2% | 50.2% | 16.1% | 11.5% |
| Embodiment 3 | 20.6% | 56.4% | 13.2% | 9.8% |
As seen from the above embodiment, the 3D printing alloy powder that preparation method provided by the invention is prepared has preferable
Mobility (flow velocity be 13.3~15.1S/50g), powder density (5.25~5.46g/cm3) be also improved, while energy
Oxygen content is enough accurately controlled below 0.018%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of 3D printing alloy powder, comprising the following steps:
Ball milling after graphene, tungsten carbide powder, cobalt powder and carbonization chromium powder are mixed, obtains mixed metal powder；
The mixed metal powder is subjected to induction plasma spheroidising, obtains 3D printing alloy powder.
2. preparation method as described in claim 1, which is characterized in that the graphene, tungsten carbide powder, cobalt powder and carbonization chromium powder
Mass ratio be (5.5~6.5): (80~95): (5~15): (0.2~0.5).
3. preparation method as described in claim 1, which is characterized in that the ball milling is wet ball grinding；
The revolving speed of the wet ball grinding is 30~36r/min, and the time of the wet ball grinding is 24~36 hours.
4. preparation method as claimed in claim 1 or 3, which is characterized in that the partial size of the mixed metal powder be 200~
300 mesh.
5. preparation method as described in claim 1, which is characterized in that after the ball milling further include: by the powder after the ball milling
Material is sieved and is dried, and mixed metal powder is obtained；The temperature of the drying is 90~95 DEG C, and the time of the drying is
2.5~4h.
6. preparation method as described in claim 1, which is characterized in that the ion-gas gas source of the induction plasma spheroidising
For Ar and H2, the Ar and H2Volume be than (22~26): 1.
7. preparation method as described in claim 1, which is characterized in that the power of the induction plasma spheroidising be 45~
60kW。
8. preparation method as described in claim 1, which is characterized in that the powder feeding rate of the induction plasma spheroidising is 5
~10kg/h.
9. the 3D printing alloy powder that preparation method according to any one of claims 1 to 8 is prepared, which is characterized in that institute
The partial size for stating 3D printing alloy powder is 45~105 μm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113737077A (en) * | 2021-09-06 | 2021-12-03 | 河源正信硬质合金有限公司 | Hard alloy with mixed crystal structure and preparation method thereof |
| CN114101663A (en) * | 2022-01-27 | 2022-03-01 | 西部宝德科技股份有限公司 | Spherical nickel powder and preparation method and application thereof |
| CN114457301A (en) * | 2021-06-28 | 2022-05-10 | 北京机科国创轻量化科学研究院有限公司 | High-speed steel self-lubricating coating and preparation method thereof |
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| CN113737077A (en) * | 2021-09-06 | 2021-12-03 | 河源正信硬质合金有限公司 | Hard alloy with mixed crystal structure and preparation method thereof |
| CN114101663A (en) * | 2022-01-27 | 2022-03-01 | 西部宝德科技股份有限公司 | Spherical nickel powder and preparation method and application thereof |
| CN114101663B (en) * | 2022-01-27 | 2022-04-15 | 西部宝德科技股份有限公司 | Spherical nickel powder and preparation method and application thereof |
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Application publication date: 20190726 |