CN114054761A - Preparation method of metal ceramic powder for 3D printing - Google Patents
Preparation method of metal ceramic powder for 3D printing Download PDFInfo
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- CN114054761A CN114054761A CN202111364199.2A CN202111364199A CN114054761A CN 114054761 A CN114054761 A CN 114054761A CN 202111364199 A CN202111364199 A CN 202111364199A CN 114054761 A CN114054761 A CN 114054761A
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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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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Abstract
The invention provides a preparation method of metal ceramic powder for 3D printing, which comprises the following steps: step S10, carrying out wet grinding mixing reaction on a composition formed by mixing TiC powder and Ni powder and a forming agent to obtain a wet grinding mixture; step S20, carrying out spray drying reaction on the wet-milled mixture to obtain a spray mixture; s30, screening the spraying mixture to obtain the spraying mixture with the target particle size; step S40, calcining the spray mixture with the target particle size in a vacuum environment to obtain metal ceramic powder; and S50, sieving the metal ceramic powder obtained in the step S40. Based on the technical scheme of the invention, the metal powder which is good in shape degree, stable in ceramic phase and suitable for 3D printing can be obtained, and the preparation method is low in cost, controllable in metal powder particle size, simple in process and convenient to produce.
Description
Technical Field
The invention relates to the technical field of powder metallurgy, in particular to a preparation method of metal ceramic powder for 3D printing.
Background
3D printing is used as a processing technology which breaks through the traditional preparation technology, is a new manufacturing technology which takes a digital model as a basis and accumulates materials layer by layer to manufacture solid objects, is suitable for design research, development and verification and the like before complex micro component products, personalized customization and large-scale production, has the advantages of high production efficiency, high material utilization rate, no need of a mold and the like, and is a hot topic which is positioned at the sharp of a wind gap internationally at present.
The existing metal powder preparation technology for 3D printing mainly comprises the following steps: mechanical crushing, atomization, chemical methods, and the like. Wherein, the mechanical crushing method is suitable for the brittle material, and the prepared powder has poor sphericity; the chemical method has higher cost and is easy to introduce toxic and harmful impurities; the atomization method is a main method for preparing metal powder for 3D printing at present, but the powder has the problems of poor satellite ball and powder flowability.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a preparation method of the metal ceramic powder for 3D printing, and the metal ceramic powder suitable for 3D printing can be obtained by mixing, granulating and performing heat treatment in a powder metallurgy mode.
The invention provides a preparation method of metal ceramic powder for 3D printing, which comprises the following steps:
step S10, carrying out wet grinding and mixing on a composition formed by mixing TiC powder and Ni powder and a forming agent to obtain a wet grinding mixture;
step S20, carrying out spray drying reaction on the wet-milled mixture to obtain a spray mixture;
s30, screening the spraying mixture to obtain the spraying mixture with the target particle size;
and step S40, calcining the spray mixture with the target particle size in a vacuum environment to obtain the metal ceramic powder.
The prepared powder has good sphericity by adopting a powder metallurgy mode, is suitable for 3D printing, and has controllable powder particle size and simple process.
In one embodiment, the spraying mixture is screened, materials with the particle size smaller than 30 μm or larger than 60 μm in the mixture are removed, and a target spraying mixture with the particle size of 30-60 μm is obtained.
In one embodiment, the present method of preparation further comprises: step S50, sieving the cermet powder obtained in step S40, and according to the present embodiment, sieving the cermet powder to remove impurities in the powder, so as to avoid affecting the quality of 3D printing.
In one embodiment, the composition comprises the following raw material materials in percentage by mass of the total composition: 20-40% of TiC powder and the balance Ni powder.
In one embodiment, the mass of the forming agent is 2 to 4% of the total mass of the composition.
In one embodiment, the forming agent is a liquid paraffin forming agent.
In one embodiment, the conditions of the wet milling mixing reaction include: the reaction time is 6-12 h.
In one embodiment, the conditions of the spray drying reaction include: the atomization pressure is 0.8-1.2 MPa.
In one embodiment, the vacuum degree of the vacuum environment is 2000-4000 Pa.
In one embodiment, the temperature of the calcination in step S40 is 1100 to 1300 ℃.
In one embodiment, in step S40, the calcination time is 1 to 3 hours.
The second aspect of the invention provides a metal ceramic powder for 3D printing, which comprises the following raw materials in parts by weight: 20-40% of TiC powder, and the balance of Ni powder.
In one embodiment, the cermet powder obtained has an average powder particle size of 30 to 60 μm and a flowability of 50g with a flow time of less than 30 seconds.
The features mentioned above can be combined in various suitable ways or replaced by equivalent features as long as the object of the invention is achieved.
Compared with the prior art, the preparation method of the metal ceramic powder for 3D printing provided by the invention at least has the following beneficial effects:
(1) the powder prepared by adopting a metal smelting mode has good and stable sphericity and is suitable for 3D printing.
(2) The preparation method has the advantages of low cost, controllable metal powder granularity and simple process.
Drawings
The invention will be described in more detail hereinafter on the basis of embodiments and with reference to the accompanying drawings. Wherein:
FIG. 1 shows a topographical view of a mixture powder after spraying in accordance with the present invention;
FIG. 2 shows a typical morphology of the cermet powder of the present invention.
Detailed Description
In order that the invention may be readily understood, a detailed description of the invention is provided below. However, before the invention is described in detail, it is to be understood that this invention is not limited to particular embodiments described. It is also to be understood that the terminology used herein is for the purpose of describing particular embodiments only, and is not intended to be limiting.
Where a range of values is provided, it is understood that each intervening value, to the extent that there is no stated or intervening value in that stated range, to the extent that there is no such intervening value, is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included in the smaller ranges, and are also encompassed within the invention, subject to any specifically excluded limit in the stated range. Where a specified range includes one or two limits, ranges excluding either or both of those included limits are also encompassed by the invention.
Unless otherwise defined, all terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although any methods and materials similar or equivalent to those described herein can also be used in the practice or testing of the present invention, the preferred methods and materials are now described.
As mentioned above, the existing metal powder preparation for 3D printing has the problems of high manufacturing cost, poor powder sphericity, easy generation of toxic and harmful impurities in the preparation process and the like.
Therefore, the invention provides a preparation method of metal ceramic powder for 3D printing, which comprises the following steps:
step S10, carrying out wet grinding mixing reaction on a composition formed by mixing TiC powder and Ni powder and a forming agent to obtain a wet grinding mixture;
step S20, carrying out spray drying reaction on the wet-milled mixture to obtain a spray mixture;
s30, screening the spraying mixture to obtain the spraying mixture with the target particle size;
and step S40, calcining the spray mixture with the target particle size in a vacuum environment to obtain the metal ceramic powder.
In one embodiment, in step S30, after the spray mixture is screened, the materials with the particle size smaller than 30 μm or larger than 60 μm in the mixture are removed, and the powder with the particle size of 30-60 μm, which is a graded particle size, is retained, so that the cermet powder suitable for 3D printing can be obtained in the subsequent production process.
In one embodiment, the method further comprises a step S50 of sieving the cermet powder obtained in the step S40, and removing impurities in the cermet powder through sieving to avoid affecting the quality of 3D printing.
In one embodiment, the composition comprises the following raw material materials in percentage by mass of the total composition: 20-40% of TiC powder and the balance of Ni powder.
In one embodiment, the mass of the forming agent is 2 to 4% of the total mass of the composition.
In one embodiment, the forming agent is a liquid paraffin forming agent.
In one embodiment, the conditions of the wet milling mixing reaction include: the reaction time is 6-12 h.
In one embodiment, the conditions of the spray drying reaction include: the atomization pressure is 0.8-1.2 MPa.
In one embodiment, the vacuum degree of the vacuum environment is 2000-4000 Pa.
In one embodiment, the temperature of the calcination in step S40 is 1100 to 1300 ℃.
In one embodiment, in step S40, the calcination time is 1 to 3 hours.
The invention also provides the metal ceramic powder for 3D printing and a preparation method of the metal ceramic powder for 3D printing.
In one embodiment, the cermet powder obtained has an average powder particle size of 30 to 60 μm and a flowability of 50g with a flow time of less than 30 seconds.
Examples
In order that the present invention may be more readily understood, the following detailed description will proceed with reference being made to examples, which are intended to be illustrative only and are not intended to limit the scope of the invention. The starting materials or components used in the present invention may be commercially or conventionally prepared unless otherwise specified.
Example 1:
wet-grinding and mixing 20 wt% of TiC and the balance of Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 2% of the total weight of the powder for 12 hours, carrying out spray drying on the wet-ground mixed material, carrying out spray drying under the atomization pressure of 0.8MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1100 ℃ for 3 hours for calcination under the vacuum degree of 2000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, 53 mu m of average powder particle size, oxygen content lower than 800ppm and 50g of fluidity and flow time shorter than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 2:
wet-grinding and mixing 30 wt% of TiC and the balance of Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 3% of the total weight of the powder for 9 hours, carrying out spray drying and spray drying on the wet-ground mixture under the atomization pressure of 1.0MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1200 ℃ for 2 hours for calcination under the vacuum degree of 3000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 45 mu m, the oxygen content of less than 800ppm and the fluidity of 50g for less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 3:
the preparation method comprises the following steps of wet-grinding and mixing 40 wt% of TiC and the balance Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 4% of the total weight of the powder for 6 hours, carrying out spray drying and spray drying on the wet-ground mixed material under the atomization pressure of 1.2MPa, screening the spray material to obtain powder with the particle size of 30-60 microns, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1300 ℃ for 1 hour to calcine the powder with the vacuum degree of 4000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 36 microns, the oxygen content of less than 800ppm and the fluidity of 50g for less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 4:
wet-grinding and mixing 20 wt% of TiC and the balance of Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 2% of the total weight of the powder for 12 hours, carrying out spray drying on the wet-ground mixed material, carrying out spray drying under the atomization pressure of 1.0MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1300 ℃ for 2 hours for calcination under the vacuum degree of 2000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 48 mu m, the oxygen content of less than 800ppm and the fluidity of 50g for flowing time of less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 5:
wet-grinding and mixing 30 wt% of TiC and the balance of Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 3% of the total weight of the powder for 9 hours, carrying out spray drying and spray drying on the wet-ground mixture under the atomization pressure of 1.2MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1200 ℃ for 3 hours for calcination under the vacuum degree of 3000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 37 mu m, the oxygen content of less than 800ppm and the fluidity of 50g for less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 6:
the preparation method comprises the following steps of wet-grinding and mixing 40 wt% of TiC and the balance Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 4% of the total weight of the powder for 6 hours, carrying out spray drying and spray drying on the wet-ground mixed material under the atomization pressure of 0.8MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1100 ℃ for 1 hour for calcination under the vacuum degree of 4000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 56 mu m, the oxygen content of less than 800ppm and the fluidity of 50g for less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 7:
wet-grinding and mixing 20 wt% of TiC and the balance of Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 2% of the total weight of the powder for 12 hours, carrying out spray drying on the wet-ground mixed material, carrying out spray drying under the atomization pressure of 1.2MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1200 ℃ for 1 hour for calcination under the vacuum degree of 2000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 39 mu m, the oxygen content of less than 800ppm and the fluidity of 50g for flowing time of less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 8:
wet-grinding and mixing 30 wt% of TiC and the balance of Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 3% of the total weight of the powder for 9 hours, carrying out spray drying and spray drying on the wet-ground mixture under the atomization pressure of 0.8MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1300 ℃ for 3 hours for calcination under the vacuum degree of 3000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, the average powder particle size of 51 mu m, the oxygen content of less than 800ppm and the fluidity of 50g for less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
Example 9:
the preparation method comprises the following steps of wet-grinding and mixing 40 wt% of TiC and the balance Ni powder which account for the total weight of the powder with a paraffin forming agent which accounts for 4% of the total weight of the powder for 6 hours, carrying out spray drying and spray drying on the wet-ground mixed material under the atomization pressure of 1.0MPa, screening the spray material to obtain powder with the particle size of 30-60 mu m, then carrying out heat preservation on the screened powder in a vacuum heat treatment furnace at 1100 ℃ for 2 hours to calcine the powder with the vacuum degree of 4000Pa to prepare a metal ceramic alloy composite powder aggregate, obtaining 3D printing metal ceramic powder with good sphericity, average powder particle size of 50 mu m, oxygen content of less than 800ppm and fluidity of 50g for flowing time of less than 30 seconds, and finally carrying out screening to remove impurities in the powder.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "bottom", "top", "front", "rear", "inner", "outer", "left", "right", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are only for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed in a particular orientation, and be operated, and thus, should not be construed as limiting the present invention.
Although the invention herein has been described with reference to particular embodiments, it is to be understood that these embodiments are merely illustrative of the principles and applications of the present invention. It is therefore to be understood that numerous modifications may be made to the illustrative embodiments and that other arrangements may be devised without departing from the spirit and scope of the present invention as defined by the appended claims. It should be understood that features described in different dependent claims and herein may be combined in ways different from those described in the original claims. It is also to be understood that features described in connection with individual embodiments may be used in other described embodiments.
Claims (12)
1. A preparation method of metal ceramic powder for 3D printing is characterized by comprising the following steps:
step S10, carrying out wet grinding and mixing on a composition formed by mixing TiC powder and Ni powder and a forming agent to obtain a wet grinding mixture;
step S20, carrying out spray drying reaction on the wet-milled mixture to obtain a spray mixture;
s30, screening the spraying mixture to obtain the spraying mixture with the target particle size;
and step S40, calcining the spray mixture with the target particle size in a vacuum environment to obtain the metal ceramic powder.
2. The method of preparing a cermet powder for 3D printing according to claim 1, characterized in that the target particle size is 30-60 μ ι η.
3. The method for preparing cermet powder for 3D printing according to claim 1, further comprising: and S50, sieving the metal ceramic powder obtained in the step S40.
4. The method for preparing the cermet powder for 3D printing according to claim 1, wherein the composition comprises the following raw materials in percentage by mass: 20-40% of TiC powder and the balance Ni powder.
5. The method for preparing the cermet powder for 3D printing according to claim 4, wherein the mass of the forming agent is 2-4% of the total mass of the composition.
6. The method for preparing cermet powder for 3D printing according to claim 1, characterized in that the forming agent is liquid paraffin forming agent.
7. The method for preparing cermet powder for 3D printing according to claim 1, wherein the conditions of the wet milling mixing reaction include: the reaction time is 6-12 h.
8. The method for preparing cermet powder for 3D printing according to claim 1, wherein the conditions of the spray drying reaction include: the atomization pressure is 0.8-1.2 MPa.
9. The method for preparing the cermet powder for 3D printing according to claim 1, wherein the vacuum degree of the vacuum environment is 2000 to 4000 Pa.
10. The method of preparing a cermet powder for 3D printing according to claim 1, characterized in that the calcination conditions include: the calcination temperature is 1100-1300 ℃, and the calcination time is 1-3 h.
11. The metal ceramic powder for 3D printing is characterized in that the raw materials for preparing the metal ceramic powder for 3D printing comprise the following components in parts by weight: 20-40% of TiC powder, and the balance of Ni powder.
12. The cermet powder for 3D printing according to claim 11, characterized in that the cermet powder obtained has an average particle size of 30-60 μm and a flowability of 50g and a flow time of less than 30 seconds.
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| CN115365491A (en) * | 2022-08-29 | 2022-11-22 | 浙江旗创新材料科技有限公司 | Efficient powder premixing process |
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