CN115125424B - Cermet feed for indirect 3D printing and preparation method and application thereof - Google Patents

Cermet feed for indirect 3D printing and preparation method and application thereof Download PDF

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CN115125424B
CN115125424B CN202210574291.XA CN202210574291A CN115125424B CN 115125424 B CN115125424 B CN 115125424B CN 202210574291 A CN202210574291 A CN 202210574291A CN 115125424 B CN115125424 B CN 115125424B
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powder
cermet
indirect
feed
printing
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CN115125424A (en
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郭瑜
汪强兵
郑晓川
张莹
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Guangzhou Sailong Supplementary Manufacturing Co ltd
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Guangzhou Sailong Supplementary Manufacturing Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/04—Alloys based on tungsten or molybdenum
    • 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
    • B22F1/142—Thermal or thermo-mechanical treatment
    • 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
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • 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
    • B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
    • B22F10/10—Formation of a green body
    • 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
    • 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
    • B33Y10/00—Processes of additive manufacturing
    • 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
    • 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
    • B33Y80/00—Products made by additive manufacturing
    • 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
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/06—Ceramics; Glasses; Refractories
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F1/00—Shielding characterised by the composition of the materials
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/08—Metals; Alloys; Cermets, i.e. sintered mixtures of ceramics and metals
    • G21F1/085—Heavy metals or alloys
    • 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
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/25—Process efficiency

Abstract

The invention relates to a metal ceramic feed for indirect 3D printing, which comprises metal ceramic powder and an organic bonding material, wherein the volume content of the metal ceramic powder accounts for 55-58% of the total volume of the feed; the metal ceramic powder comprises the following components in percentage by mass: 10 to 40 percent of carbide-based ceramic powder with the average grain diameter of 1 to 8 mu m and 60 to 90 percent of metal powder with the average grain diameter of 3 to 10 mu m; the metal powder is subjected to surface oxidation treatment at an oxidation temperature of 300-600 ℃; the organic bonding material includes at least two different binders. The powder loading capacity of the metal ceramic feeding material for indirect 3D printing is higher than that of the traditional metal ceramic feeding material for indirect 3D printing, the feeding viscosity is appropriate after the organic bonding material is heated to reach the melting temperature during 3D printing, and the nuclear radiation shielding product obtained by 3D printing is high in quality stability.

Description

Metal ceramic feed for indirect 3D printing and preparation method and application thereof
Technical Field
The invention relates to the technical field of 3D printing, in particular to a metal ceramic feed for indirect 3D printing and a preparation method and application thereof.
Background
With the increasing problem of energy shortage, nuclear technology has been greatly developed. However, various radiation rays are generated in the nuclear energy system, and the nuclear radiation rays are very harmful to the environment and the human body. Therefore, research on nuclear radiation shielding materials has received much attention in the nuclear industry.
For example, boron carbide has high neutron absorption capacity, good corrosion resistance and good thermal stability, is an ideal neutron shielding material, is compounded and mixed with tungsten powder to form a boron carbide-tungsten composite material, and the composite material not only can improve the hardness and the thermal stability of the material, but also can effectively shield neutrons and gamma rays of a nuclear reactor and is beneficial to the attenuation effect of the gamma rays, so that the boron carbide-tungsten composite material is a nuclear radiation shielding material with great application potential. However, the conventional mixing-molding technique has great limitation, and is difficult to prepare into the product with high B 4 C content nuclear radiation shielding articles, and therefore, how to make nuclear radiation shielding articles based on boron carbide-tungsten composites is a focus of research in nuclear industry applications.
The indirect 3D printing technology based on adhesive bonding is a new method for manufacturing complex metal ceramic materials, the 3D forming process of the method is to mix a high molecular polymer adhesive and metal ceramic powder according to a certain proportion to prepare a uniform mixed material with good fluidity, namely 3D printing feed, then the feed is extruded at the melting temperature of the adhesive, and layer-by-layer deposition is carried out according to a digital 3D model, and finally a 3D printing blank body can be obtained. The key of the indirect 3D printing and forming process is that the added binder has good adsorbability on the metal ceramic powder, so that the binding force between the metal ceramic powder and the binder can be greatly enhanced, and the metal ceramic powder is finally formed into parts with complex shapes through fusion deposition.
The boron carbide-tungsten composite is also a cermet material, and therefore, the indirect 3D printing technology is a method which has high feasibility and can be used for manufacturing nuclear radiation shielding products based on the boron carbide-tungsten composite. However, the indirect 3D printing has a great difficulty in manufacturing a nuclear radiation shielding product based on a boron carbide-tungsten composite material, and the reason is mainly that in the process of refining the 3D printing feed, the binder is difficult to wet the boron carbide and the metal tungsten powder at the same time, so that the boron carbide-tungsten composite powder in the feed has poor dispersibility and low powder loading capacity, and the quality of a product obtained by 3D printing with the feed is unstable.
Disclosure of Invention
Based on the above, there is a need for a cermet feed for indirect 3D printing, which can improve the dispersibility and powder loading of cermet powder in the feed and can improve the stability of 3D printing quality, and a preparation method and applications thereof.
The invention provides a metal ceramic feed for indirect 3D printing, which comprises metal ceramic powder and an organic bonding material, wherein the volume content of the metal ceramic powder accounts for 55-58% of the total volume of the feed;
the metal ceramic powder comprises the following components in percentage by mass:
10 to 40% of carbide-based ceramic powder having an average particle diameter of 1 to 8 μm, and
60 to 90 percent of metal powder with the average grain diameter of 3 to 10 mu m;
the metal powder is subjected to surface oxidation treatment at an oxidation temperature of 300-600 ℃;
the organic bonding material includes at least two different binders.
In one embodiment, the metal powder is subjected to surface oxidation treatment, which comprises the following steps:
and heating the metal powder to the oxidation temperature at the speed of 2-5 ℃/min in an oxygen-containing atmosphere, and keeping the temperature for 10-30 min.
In one embodiment, the oxygen-containing atmosphere is provided by introducing an oxygen-containing gas under the following conditions: the total gas flow is 50 sccm/min-200 sccm/min, and the proportion of the oxygen flow in the total gas flow is 1 (3-12).
In one embodiment, the material of the carbide-based ceramic powder is at least one of boron carbide, titanium carbide and molybdenum carbide; and/or
The material of the metal powder is at least one of tungsten and molybdenum; and/or
The average grain diameter of the carbide-based ceramic powder is 3-8 mu m; and/or
The average particle diameter of the metal powder is 5-8 μm.
In one embodiment, the organic binding material comprises the following components in percentage by mass:
55 to 75 percent of filling agent,
20% to 38% of a binder, and
1 to 8 percent of dispersant.
In one embodiment, the organic binding material comprises the following components in percentage by mass:
58 to 65 percent of filler,
30 to 36% of a binder, and
3 to 6 percent of dispersant.
In one embodiment, the filler is at least one of carnauba wax, microcrystalline wax, sliced paraffin wax, and polyethylene wax; and/or
The binder is at least two of high-density polyethylene, polypropylene, polystyrene and ethylene-vinyl acetate copolymer; and/or
The dispersant is at least one of stearic acid, zinc stearate, phthalate and salad oil.
In one embodiment, the binder in the organic binding material comprises 20-38% by mass of high density polyethylene and 0-18% by mass of polypropylene.
The invention also provides a preparation method of the cermet feed for indirect 3D printing, which comprises the following steps:
mixing the carbide-based ceramic powder and the metal powder subjected to surface oxidation treatment according to a preset volume content to prepare the metal ceramic powder;
and mixing the metal ceramic powder and the organic bonding material, and granulating.
In one embodiment, in the step of preparing the cermet powder, the mixing includes:
ball-milling the mixture of the carbide-based ceramic powder and the metal powder, wherein the ball-milling medium is absolute ethyl alcohol, ball-milling the mixture for 6 to 12 hours at the rotating speed of between 90 and 120r/min, and sieving the mixture with 200 to 500 meshes after the ball-milling is finished; and/or
The process of mixing the cermet powder with the organic binder material comprises the following steps:
mixing at 140-170 deg.c for 30-60 min; and/or
The nozzle temperature of the granulating device used in granulation is 130-160 ℃, and the screw temperature is 140-165 ℃.
The invention also provides a preparation method of the nuclear radiation shielding product, which comprises the following steps:
3D printing was performed using a cermet feed for indirect 3D printing as described in any of the examples above.
The invention also provides a nuclear radiation shielding product prepared by the preparation method of the nuclear radiation shielding product.
According to the metal ceramic feed for indirect 3D printing, the metal powder is subjected to surface oxidation treatment, so that the organic bonding material has good affinity to the metal powder and the carbide-based ceramic powder, the dispersion performance of the metal ceramic powder in the organic bonding material can be obviously improved, the volume content of the metal ceramic powder in the feed can reach 55% -58%, the volume content of the metal ceramic powder is higher than that of the traditional metal ceramic feed for indirect 3D printing, the feed is proper in viscosity after the metal ceramic powder is heated to the melting temperature of the organic bonding material during 3D printing, and the nuclear radiation shielding product obtained by 3D printing is high in quality stability.
Drawings
FIG. 1 is a photograph of the topography of a cermet feed for indirect 3D printing according to one embodiment;
FIG. 2 is an SEM scan of a cermet powder used to prepare a cermet feedstock for indirect 3D printing of an example;
FIG. 3 is a photograph of an embodiment of an indirect 3D printing cermet feed for 3D printing;
FIG. 4 is an SEM scan of the cermet feedstock for indirect 3D printing of example 1;
FIG. 5 is an SEM scan of the cermet feedstock for indirect 3D printing of example 2;
FIG. 6 is an SEM scan of the cermet feedstock for indirect 3D printing of example 3;
FIG. 7 is an SEM scan of the cermet feedstock for indirect 3D printing of comparative example 1;
FIG. 8 is an SEM scan of a cermet feedstock for indirect 3D printing of comparative example 2;
FIG. 9 is an SEM scan of the cermet feedstock for indirect 3D printing of comparative example 3;
fig. 10 is an SEM scan of the cermet feedstock for indirect 3D printing of comparative example 4.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the present invention, the technical features described in the open type include a closed technical solution composed of the listed features, and also include an open technical solution including the listed features.
As shown in fig. 1 and in combination with fig. 2, an embodiment of the present invention provides a cermet feed for indirect 3D printing, including a cermet powder and an organic binder, wherein the volume content of the cermet powder is 55% to 58% of the total volume of the feed.
The metal ceramic powder comprises the following components in percentage by mass:
10 to 40% of carbide-based ceramic powder having an average particle diameter of 1 to 8 μm, and
60 to 90 percent of metal powder with the average grain diameter of 3 to 10 mu m.
The carbide-based ceramic material is a material with neutron absorption performance and radiation resistance, and is a good radiation shielding material, the metal material also has the effect of nuclear radiation shielding and has higher strength, the carbide-based ceramic material and the metal material are combined to form the cermet material, the nuclear radiation shielding effect of the carbide-based ceramic material and the metal material can be enhanced, the hardness and the thermal stability of the material can be improved, in addition, the cermet material can be further prepared into a nuclear radiation shielding product with high cermet content by utilizing an indirect 3D printing technology, and the problem that the nuclear radiation shielding product with high cermet content is difficult to prepare in the traditional mixing-die pressing technology is solved.
The organic bonding material in the metal ceramic feed for indirect 3D printing has very good affinity performance to metal ceramic powder, and the metal ceramic powder is uniformly distributed in the organic bonding material and has good dispersion performance. Further, since the dispersion of the cermet powder in the feed material is good, the powder loading can be further increased, and it is understood that the powder loading herein refers to the volume content of the cermet powder in the feed material. Furthermore, the method is favorable for preparing the feed with high cermet content, and further preparing the nuclear radiation shielding product with high cermet content, and further can further improve the nuclear radiation shielding effect of the nuclear radiation shielding product.
Further, the metal powder in the embodiment of the present invention is surface-oxidized at an oxidation temperature of 300 to 600 ℃. The metal powder is subjected to surface oxidation treatment so that the metal surface contains oxygen atoms, and the metal and oxygen atoms are covalently bonded in the same manner as the atoms of the carbide-based ceramic powder, and the bonding characteristics thereof with the organic binder are the same, whereby the dispersibility of the metal ceramic powder in the organic binder is improved.
In one embodiment of the present invention, a method for performing surface oxidation treatment on metal powder is provided, which specifically includes the following steps:
the metal powder is heated to the oxidation temperature of 300-600 ℃ at the speed of 2-5 ℃/min in the oxygen-containing atmosphere, and the temperature is kept for 10-30 min.
Further, an oxygen-containing atmosphere is provided by introducing an oxygen-containing gas under the following conditions: the total gas flow is 50 sccm/min-200 sccm/min, and the proportion of the oxygen flow in the total gas flow is 1 (3-12). The convection exchange of gas in the reaction system can be accelerated by continuously introducing flowing gas, the metal surface oxidation treatment efficiency is favorably improved, the oxidation effect is more uniform, and the oxidation degree is more easily controlled. Furthermore, by controlling the oxygen content in the flowing gas, the surface of the metal powder can realize a good oxidation effect but can not be excessively oxidized, and the phenomenon that the oxidation is excessive to cause an oxide film formed on the surface of the metal powder to be too rough is avoided, so that the capability of the metal powder for absorbing neutron radiation is reduced.
Further, the aeration conditions were: the total gas flow is 50 sccm/min-200 sccm/min, and the proportion of the oxygen flow in the total gas flow is 1 (4-6).
It will be appreciated that the flow gas may be supplied with a protective gas, such as nitrogen, argon, etc., in addition to oxygen.
Further, the flowing gas is a mixed flowing gas composed of oxygen and nitrogen, and the aeration conditions are as follows: the total gas flow is 50 sccm/min-200 sccm/min, and the proportion of the oxygen flow in the total gas flow is 1 (4-6).
Furthermore, the oxidation temperature is 350-400 ℃.
In a specific example, the material of the carbide-based ceramic powder may be, for example, but not limited to, at least one of boron carbide, titanium carbide, and molybdenum carbide.
In a specific example, the material of the metal powder may be, but is not limited to, at least one of tungsten and molybdenum.
In a specific example, the average particle size of the carbide-based ceramic powder is 3 μm to 8 μm.
In a specific example, the metal powder has an average particle diameter of 5 μm to 8 μm.
In a specific example, the organic binding material comprises the following components in percentage by mass:
55 to 75 percent of filling agent,
20% to 38% of a binder, and
1 to 8 percent of dispersant.
It can be understood that the composition and the amount of the organic bonding material are important factors determining rheological properties of the cermet feeding material for indirect 3D printing, the filler in the organic bonding material is used for wrapping particles of the cermet powder, which is beneficial to improving the flowability of the feeding material, the binder is used for improving the strength of a 3D printing forming blank, the dispersant is used for improving the dispersibility of the cermet powder and the binder, and the filler, the binder and the dispersant are mixed according to a proper mass ratio to form the organic bonding material, so that the feeding material can be further ensured to have proper viscosity during 3D printing, and further, the quality stability of the printed nuclear radiation shielding product is ensured to be higher.
Further, the organic binding material comprises the following components in percentage by mass:
58 to 65 percent of filler,
30% to 36% of a binder, and
3 to 6 percent of dispersant.
Wherein the organic bonding material comprises at least two different bonding agents, such as but not limited to at least two of high density polyethylene, polypropylene, polystyrene, and ethylene-vinyl acetate copolymer. In the organic bonding material, the composite bonding agent composed of at least two different bonding agents is adopted, so that the bonding strength between the metal ceramic powder and the organic bonding material is favorably improved, and the 3D printing quality is favorably improved.
Preferably, the binder in the organic binding material comprises 20-38% by mass of high density polyethylene and 0-18% by mass of polypropylene. The composite binder formed by mixing the high-density polyethylene and the polypropylene according to a specific mass ratio can enable the feed to have better high-temperature flow performance, and the high-density polyethylene and the polypropylene are matched according to a specific mass ratio to form the composite binder, so that the bonding strength of the composite binder and the metal ceramic powder is better than that of a single binder, and the composite binder is favorable for obtaining a printing blank with better tissue dispersibility.
Preferably, the binder in the organic binding material comprises 25 to 26% by mass of high density polyethylene and 5 to 10% by mass of polypropylene.
Further, the filler may be, for example, but not limited to, at least one of carnauba wax, microcrystalline wax, sliced paraffin wax, and polyethylene wax.
Further, the dispersant may be, for example, but not limited to, at least one of stearic acid, zinc stearate, phthalate, and salad oil.
An embodiment of the present invention further provides a method for preparing a cermet feed for indirect 3D printing as in any one of the above examples, comprising the steps of:
the method comprises the following steps: and mixing the carbide-based ceramic powder and the metal powder subjected to surface oxidation treatment according to a preset volume content to prepare the metal ceramic powder.
Specifically, the process of mixing includes:
ball milling is carried out on the mixture of the carbide-based ceramic powder and the metal powder, the ball milling medium is absolute ethyl alcohol, ball milling is carried out for 6 h-12 h at the rotating speed of 90 r/min-120 r/min, and the mixture is sieved by 200 meshes-500 meshes after the ball milling is finished.
Understandably, through the mode of ball-milling, can be with carbide base ceramic powder and the metal powder intensive mixing who carries out surface oxidation treatment even, and can further reduce the particle diameter of powder, be favorable to the in-process of follow-up mixing again, make the distribution of these two kinds of different powders of carbide base ceramic powder and metal powder more even in organic bonding material system, promote the dispersion effect of powder.
Step two: mixing the metal ceramic powder and the organic binding material, and granulating.
Specifically, the mixing process comprises the following steps: mixing at 140-170 deg.c for 30-60 min.
Specifically, the nozzle temperature of the granulation apparatus used for granulation is 130 to 160 ℃ and the screw temperature is 140 to 165 ℃.
When the metal ceramic powder and the organic bonding material are mixed, the metal powder is subjected to surface oxidation treatment, the metal ceramic powder is composed of carbide-based ceramic powder with a specific particle size and the metal powder according to a specific mass ratio, the organic bonding material and the metal ceramic powder have good affinity, the organic bonding material is in a molten state during mixing, and the capillary force between the organic bonding material and the metal ceramic powder is increased, so that the organic bonding material can more easily go deep into clusters of the metal ceramic powder, a physical form that the metal ceramic powder is wrapped by the organic bonding material is formed, and the dispersion performance of the metal ceramic powder in the organic bonding material is improved. Further, the volume content of the metal ceramic powder is improved, the volume content of the metal ceramic powder in the feed can reach 55-58%, and understandably, the volume content of the metal ceramic powder in the feed is the powder loading amount of the feed.
As shown in fig. 3, the present invention also provides a method for preparing a nuclear radiation shielding article, comprising the steps of:
3D printing was performed using a cermet feed for indirect 3D printing as in any of the examples above.
It is to be understood that the 3D printing method in this embodiment may employ an indirect 3D method that is conventional in the art. It is understood that the 3D printing method comprises at least the following three steps:
the method comprises the following steps: the cermet feed for indirect 3D printing as in any one of the examples above is loaded into an indirect 3D printing apparatus.
Step two: after heating the organic binder material to a melt temperature, the feedstock is extruded.
Step three: and carrying out layer-by-layer deposition according to a preset digital 3D model to form a 3D printing blank of the nuclear radiation shielding product.
It will be appreciated that the melting temperature is related to the specific composition and content of the organic binding material. In one specific example, the melting temperature is 150 ℃ to 160 ℃.
In one specific example, the feed is extruded at a shear rate of 100s -1 ～1000s -1 。
In a specific example, the viscosity at the time of printing is 50Pa · s to 200Pa · s.
The invention also provides a nuclear radiation shielding product which is prepared by the preparation method of the nuclear radiation shielding product.
The following are specific examples. In the following specific examples, all starting materials are commercially available unless otherwise specified.
Wherein the boron carbide powder is purchased from Shanghai Allantin Biotechnology GmbH with model number T140784;
tungsten powder, purchased from shores carbide limited, model FW-1;
carnauba wax, available from Shanghai Allantin Biotechnology GmbH, model number C104040;
high density polyethylene, available from haman plastics ltd, suzhou, model number DMDA8008;
the polypropylene is purchased from Shanghai area chemical industry Co., ltd, and has the model of PPB-M02-G;
stearic acid, model number 1801, available from silver chemical Limited, guangzhou.
Example 1
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 3 μm; tungsten powder having an average particle diameter of 5 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
The organic bonding material comprises the following components: the filler is carnauba wax, the binder is high-density polyethylene and polypropylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: polypropylene: stearic acid =65%:25%:6%:4 percent.
Feeding, mixing and feeding proportion: 55% of metal ceramic powder by volume and 45% of organic binding material by volume.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 400 ℃ at the speed of 3 ℃/min under the condition of ventilation, and preserving heat for 20min; and (3) aeration conditions: the gas flow ratio of oxygen to nitrogen is 1:4, the gas flow rate is 120sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring the boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 12 hours at the rotating speed of 90r/min, and sieving the powder with a 300-mesh sieve after the ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 160 ℃ for 45min; and then putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 150 ℃, and the screw temperature is 155 ℃.
Example 2
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 5 μm; tungsten powder having an average particle diameter of 8 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
The organic bonding material comprises the following components: the filler is carnauba wax, the binder is high-density polyethylene and polypropylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: polypropylene: stearic acid =58%:26%:10%:6 percent.
Feeding, mixing and feeding proportioning: 58% of the volume content of the metal ceramic powder and 42% of the volume content of the organic binding material.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 350 ℃ at the speed of 2 ℃/min under the condition of ventilation, and preserving heat for 30min; and (3) aeration conditions: the gas flow ratio of oxygen to nitrogen is 1:4, the gas flow rate was 150sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 6 hours at the rotating speed of 120r/min, and sieving the powder with a 200-mesh sieve after the ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 170 ℃ for 50min; and then putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 160 ℃, and the screw temperature is 165 ℃.
Example 3
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 8 μm; tungsten powder having an average particle diameter of 6 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
Organic bonding material composition: the filler is carnauba wax, the binder is high-density polyethylene and polypropylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: polypropylene: stearic acid =65%:25%:6%:4 percent.
Feeding, mixing and feeding proportioning: 57% of the volume content of the metal ceramic powder and 43% of the volume content of the organic binding material.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 400 ℃ at the speed of 3 ℃/min under the condition of ventilation, and preserving heat for 20min; and (3) aeration conditions: the gas flow ratio of oxygen to nitrogen is 1:4, the gas flow rate is 120sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 12 hours at a rotating speed of 90r/min, and sieving the powder with a 200-mesh sieve after ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 160 ℃ for 45min; and then putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 150 ℃, and the screw temperature is 155 ℃.
Comparative example 1
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 1 μm; tungsten powder having an average particle diameter of 15 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
Organic bonding material composition: the filler is carnauba wax, the binder is high-density polyethylene and polypropylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: polypropylene: stearic acid =65%:25%:6%:4 percent.
Feeding, mixing and feeding proportion: 55% of metal ceramic powder by volume and 45% of organic binding material by volume.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 400 ℃ at the speed of 3 ℃/min under the condition of ventilation, and preserving heat for 20min; and (3) aeration conditions: the flow ratio of oxygen to nitrogen is 1:4, the gas flow rate is 120sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring the boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 12 hours at the rotating speed of 90r/min, and sieving the powder with a 300-mesh sieve after the ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 160 ℃ for 45min; and then putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 150 ℃, and the screw temperature is 155 ℃.
Comparative example 2
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 5 μm; tungsten powder having an average particle diameter of 8 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
Organic bonding material composition: the filler is carnauba wax, the binder is high-density polyethylene and polypropylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: polypropylene: stearic acid =58%:26%:10%:6 percent.
Feeding, mixing and feeding proportion: 53% of metal ceramic powder and 47% of organic binding material.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 350 ℃ at the speed of 2 ℃/min under the ventilation condition, and preserving heat for 30min; and (3) aeration conditions: the flow ratio of oxygen to nitrogen is 1:4, the gas flow rate is 150sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 6 hours at the rotating speed of 120r/min, and sieving the powder with a 200-mesh sieve after the ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 170 ℃ for 50min; and then putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 160 ℃, and the screw temperature is 165 ℃.
Comparative example 3
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 5 μm; tungsten powder having an average particle diameter of 8 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
The organic bonding material comprises the following components: the filler is carnauba wax, the binder is high-density polyethylene and polypropylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: polypropylene: stearic acid =58%:26%:10%:6 percent.
Feeding, mixing and feeding proportioning: 58% of volume content of metal ceramic powder and 42% of volume content of organic binding material.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 280 ℃ at the speed of 2 ℃/min under the condition of ventilation, and preserving heat for 30min; and (3) aeration conditions: the gas flow ratio of oxygen to nitrogen is 1:4, the gas flow rate is 150sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 6 hours at the rotating speed of 120r/min, and sieving the powder with a 200-mesh sieve after the ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 170 ℃ for 50min; and then, putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 160 ℃, and the screw temperature is 165 ℃.
Comparative example 4
1. The formula is as follows:
cermet powder composition: boron carbide powder having an average particle diameter of 8 μm; tungsten powder having an average particle diameter of 6 μm. The mass percentage is as follows: boron carbide powder: tungsten powder =20%:80 percent.
The organic bonding material comprises the following components: the filler is carnauba wax, the binder is high-density polyethylene, and the dispersant is stearic acid. The mass percentage is as follows: carnauba wax: high density polyethylene: stearic acid =61%:35 percent: 4 percent.
Feeding, mixing and feeding proportion: 57% of the volume content of the metal ceramic powder and 43% of the volume content of the organic binding material.
2. Preparation:
(1) Surface oxidation treatment of metal powder: placing tungsten powder in a burning dish, heating to 400 ℃ at the speed of 3 ℃/min under the ventilation condition, and preserving heat for 20min; and (3) aeration conditions: the gas flow ratio of oxygen to nitrogen is 1:4, the gas flow rate is 120sccm/min.
(2) Preparing metal ceramic powder: and (2) pouring boron carbide powder and the tungsten powder subjected to surface oxidation treatment in the step (1) into a ball milling tank with a ball milling medium of absolute ethyl alcohol for ball milling for 12 hours at a rotating speed of 90r/min, and sieving the powder with a 200-mesh sieve after ball milling is finished.
(3) Preparing and feeding: pouring the metal ceramic powder obtained in the step (2) into a preheated internal mixer, adding an organic bonding material according to a feeding ratio, and mixing the metal ceramic powder and the organic bonding material at the mixing temperature of 160 ℃ for 45min; and then putting the mixed product into a granulator for granulation, wherein the nozzle temperature of the granulator is 150 ℃, and the screw temperature is 155 ℃.
SEM spectrogram scanning was performed on the cermet feedstock for indirect 3D printing prepared in examples 1 to 3 and comparative examples 1 to 4, and the scanning results are shown in fig. 4 to 10, in which:
fig. 4 to 6 show SEM spectra of the cermet feeds for indirect 3D printing of examples 1 to 3, in which all the powder particles were uniformly coated with the binder, the original surface of the powder was not exposed, and it can be seen that the boron carbide and tungsten powders in the feeds were uniformly dispersed in the organic binder material system.
Fig. 7 to 10 show SEM spectra of the cermet feeds for indirect 3D printing in comparative examples 1 to 4, in which the binder only covers a part of the particles, and the binder is locally aggregated, and a part of the powder particles are detached from the binder adhesion, and it can be seen that the boron carbide and tungsten powder in the feed are difficult to be uniformly dispersed in the organic binder material system.
The actual powder loading in the cermet feeds for indirect 3D printing prepared in examples 1 to 3 and comparative examples 1 to 4 was tested by the following test methods: extruding a certain mass of feed material by a feed extruder, and measuring the volume and mass of the feed material to obtain the real density of the feed material; and then, converting the density of the powder in the feeding process and the theoretical density of the binder to obtain a numerical value of the actual powder loading capacity.
The viscosity and the indirect 3D printing stability of the cermet feeds for indirect 3D printing prepared in examples 1 to 3 and comparative examples 1 to 4 were tested, and the test methods were as follows:
viscosity test upon 3D printing: the corresponding viscosity value can be quantitatively converted by calculating through a Hagen-Poiseuille equation and measuring the feeding extrusion flow of the extrusion screw of the printer under the printing specific process parameters; i.e., the greater the volumetric flow rate of the extrusion feed, the lower the viscosity.
Stability testing of indirect 3D printing: and (3) carrying out statistics on the feeding extrusion flow for 10 minutes, wherein the quality of the extruded feeding is not more than 2%, the quality of the extruded feeding is not more than 5%, and the quality of the extruded feeding is not less than 5%.
The actual powder loading, viscosity at the time of 3D printing, and indirect 3D printing stability test results of examples 1 to 3 and comparative examples 1 to 4 are shown in table 1 below.
TABLE 1 actual powder loading, viscosity during 3D printing, indirect 3D printing stability test results
Figure BDA0003661461200000191
All possible combinations of the technical features of the above embodiments may not be described for the sake of brevity, but should be considered as within the scope of the present disclosure as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is specific and detailed, but not to be understood as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.

Claims (12)

1. The cermet feed for indirect 3D printing is characterized by comprising cermet powder and an organic bonding material, wherein the volume content of the cermet powder in the feed is 55-58%;
the metal ceramic powder comprises the following components in percentage by mass:
10 to 40% of carbide-based ceramic powder having an average particle diameter of 1 to 8 μm, and
60 to 90 percent of metal powder with the average grain diameter of 3 to 10 mu m;
the metal powder is subjected to surface oxidation treatment at an oxidation temperature of 300-600 ℃;
the organic binder material includes at least two different binders.
2. The cermet feed for indirect 3D printing according to claim 1, wherein the surface oxidation treatment of the metal powder comprises the following steps:
and heating the metal powder to the oxidation temperature at the speed of 2-5 ℃/min in the oxygen-containing atmosphere, and keeping the temperature for 10-30 min.
3. The cermet feed for indirect 3D printing according to claim 2, characterized in that the oxygen containing atmosphere is provided by feeding oxygen containing gas under the following conditions: the total gas flow is 50 sccm/min-200 sccm/min, and the proportion of the oxygen flow in the total gas flow is 1 (3-12).
4. The cermet feed for indirect 3D printing according to any of claims 1-3, characterized in that the material of the carbide-based ceramic powder is at least one of boron carbide, titanium carbide and molybdenum carbide; and/or
The material of the metal powder is at least one of tungsten and molybdenum; and/or
The average grain diameter of the carbide-based ceramic powder is 3-8 mu m; and/or
The average particle diameter of the metal powder is 5-8 μm.
5. The cermet feed for indirect 3D printing according to any of claims 1-3, characterized in that the organic binding material comprises the following components in mass percent:
55 to 75 percent of filling agent,
20% to 38% of a binder, and
1 to 8 percent of dispersant.
6. The cermet feed for indirect 3D printing according to claim 5, wherein the organic binding material comprises the following components in percentage by mass:
58 to 65 percent of filler,
30 to 36% of a binder, and
3 to 6 percent of dispersant.
7. The cermet feed for indirect 3D printing according to claim 5, wherein the filler is at least one of carnauba wax, microcrystalline wax, sliced paraffin wax and polyethylene wax; and/or
The binder is at least two of high-density polyethylene, polypropylene, polystyrene and ethylene-vinyl acetate copolymer; and/or
The dispersant is at least one of stearic acid, zinc stearate, phthalate and salad oil.
8. The cermet feed for indirect 3D printing according to claim 7, characterised in that the binder in the organic binder material comprises 20-38% high density polyethylene and 0-18% polypropylene, in mass%.
9. A method of preparing a cermet feed for indirect 3D printing according to any of claims 1 to 8, characterized in that it comprises the following steps:
mixing the carbide-based ceramic powder and the metal powder subjected to surface oxidation treatment according to a preset volume content to prepare the metal ceramic powder;
and mixing the metal ceramic powder and the organic bonding material, and granulating.
10. The method for preparing a cermet feed for indirect 3D printing according to claim 9 wherein in the step of preparing the cermet powder, the mixing process comprises:
ball-milling the mixture of the carbide-based ceramic powder and the metal powder, wherein the ball-milling medium is absolute ethyl alcohol, ball-milling the mixture for 6 to 12 hours at the rotating speed of between 90 and 120r/min, and sieving the mixture with 200 to 500 meshes after the ball-milling is finished; and/or
The process of mixing the cermet powder with the organic binder material includes:
mixing at 140-170 deg.c for 30-60 min; and/or
The nozzle temperature of the granulating device used in granulation is 130-160 ℃, and the screw temperature is 140-165 ℃.
11. A method of making a nuclear radiation shielding article, comprising the steps of:
3D printing is performed using the cermet feed for indirect 3D printing as claimed in any one of claims 1 to 8.
12. A nuclear radiation shielding article produced by the method of producing a nuclear radiation shielding article according to claim 11.
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