CN111659881B - Tungsten-based radiation protection composite material for additive manufacturing and preparation method thereof - Google Patents
Tungsten-based radiation protection composite material for additive manufacturing and preparation method thereof Download PDFInfo
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- CN111659881B CN111659881B CN202010603319.9A CN202010603319A CN111659881B CN 111659881 B CN111659881 B CN 111659881B CN 202010603319 A CN202010603319 A CN 202010603319A CN 111659881 B CN111659881 B CN 111659881B
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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
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/001—Starting from powder comprising reducible metal compounds
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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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- 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
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Abstract
The invention discloses a tungsten-based radiation protection composite material for additive manufacturing and a preparation method thereof, wherein the tungsten-based radiation protection composite material comprises the following raw materials: the preparation method comprises the steps of S1, mixing the tungsten material and the grafting treating agent according to the formula amount, and carrying out grafting reaction to obtain a product A; s2, adding the thermoplastic resin with the formula amount into the product A, and mixing to obtain a product B; s3, adding the antioxidant, the plasticizer and the softener in the formula amount into the product B in sequence, and mixing to obtain a product C; s4, adding a reducing agent and an activating agent into the product C, and mixing and gelling to obtain a product D; s5, extruding and molding the product D to obtain the tungsten-based radiation protection composite material. The tungsten-based radiation protection composite material prepared by the invention has high density, high shielding efficiency and high plasticity, is suitable for the SLM technology, and solves the problem that the tungsten-based radiation protection material is difficult to form and process.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing composite materials, and particularly relates to a tungsten-based radiation protection composite material for additive manufacturing and a preparation method thereof.
Background
With the rapid development of nuclear technology in national defense and civil industries, various high-energy particles, such as alpha particles, beta particles, gamma rays, X rays, neutrons, protons and the like are widely applied to the fields of national defense and military, aviation and navigation, industrial exploration, medical treatment and health, wireless communication, science and technology and the like, thereby promoting the civilized development of human beings and burying radiation potential safety hazards. Therefore, shielding and protecting high-energy particle radiation is the key point for eliminating hidden danger, the application and development of radiation protection materials are particularly important, and the demand of the radiation protection materials is more and more increased. The tungsten-containing material is the most excellent high-energy ray shielding material, has excellent attenuation and absorption capacity on x-ray, gamma-ray and radioisotope radiation, is more than 40% higher than that of the common lead, has the characteristics of high elastic modulus, high thermal shock resistance, low thermal expansion coefficient, good high-temperature strength and the like, can meet the protection under extreme conditions (high temperature and radiation environments, namely electrons, protons, neutrons and alpha particles), and is widely applied to the fields of medical diagnosis and treatment, nuclear energy utilization, article security inspection, industrial flaw detection and the like. Tungsten materials are becoming the research direction and development trend as the shielding materials of the new generation.
However, metal tungsten has characteristics such as high hardness, high melting point, and brittleness, which makes the forming process difficult and tends to be limited in shape when applied. The tungsten-based alloy is mostly prepared by a powder metallurgy method, a die is needed in the preparation process, the preparation time of the die is long, the process is complicated, and the requirement on powder is strict. The additive manufacturing technology can realize rapid prototype manufacturing of parts, integral manufacturing of complex-shaped structures, material saving, cost reduction, production period shortening, part joint elimination and part service life improvement, and is an optimal preparation technology for tungsten-based radiation protection materials.
CN201810868684.5 discloses a tungsten/PEEK radiation protection composite material for 3D printing and a preparation method thereof, which uses tungsten powder, plasticizer and titanate coupling agent as raw materials, and cn201810868685.x discloses a SEBS-coated metal tungsten 3D printing composite material and a preparation method thereof, which uses SEBS and tungsten powder as raw materials.
Disclosure of Invention
In order to solve the technical problems, the invention provides a tungsten-based radiation protection composite material for additive manufacturing and a preparation method thereof, the prepared tungsten-based radiation protection composite material has high density, high shielding efficiency and high plasticity, is suitable for Selective Laser Melting (SLM), and a workpiece printed by the SLM has good radiation protection and comprehensive mechanical properties of tungsten alloy, and has wide application.
In order to achieve the purpose, the invention adopts the following technical scheme:
a tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials: tungsten material, grafting treating agent, thermoplastic resin, anti-aging agent, plasticizer, softening agent, reducing agent and activating agent.
Preferably, the tungsten material is at least one of tungsten powder, tungsten carbide powder and tungsten oxide.
Preferably, the particle size of the tungsten powder and the tungsten carbide powder is 1-150 μm; the tungsten oxide is nano-scale tungsten oxide.
Preferably, the grafting treatment agent is at least one of a silane coupling agent, a titanate coupling agent, and a carboxylic acid type chelating agent.
Preferably, the thermoplastic resin is at least one of natural rubber, synthetic rubber, reclaimed rubber, nylon and polypropylene; more preferably at least one of butyl rubber and nylon.
Preferably, the anti-aging agent is at least one of ketoamine, anti-aging agent D, anti-aging agent 4010 and anti-aging agent 264.
Preferably, the plasticizer is at least one of stearic acid, zinc oxide and acrylate copolymer; further preferably at least one of stearic acid and zinc oxide.
Preferably, the softening agent is at least one of a pine oil system, a petroleum system, a coal tar system, and a fatty oil system.
Preferably, the reducing agent is at least one of cobalt powder, nickel powder, magnesium powder, silver powder, aluminum powder and iron powder.
Preferably, the activating agent is at least one of sodium fluoride, sodium chloride, sodium nitrate and sodium sulfite.
Preferably, the tungsten-based radiation protection composite material for additive manufacturing comprises the following raw materials in percentage by weight: 70-96% of tungsten material, 0.01-1% of grafting treatment agent, 2-6% of thermoplastic resin, 0.01-1% of anti-aging agent, 0.01-1% of plasticizer, 0.01-1% of softening agent, 1.4-25% of reducing agent and 0.5-1% of activator.
The invention also provides a preparation method of the tungsten-based radiation protection composite material for additive manufacturing, which comprises the following steps:
s1, mixing the tungsten material and the grafting treatment agent according to the formula ratio, uniformly stirring, and stirring at 60-200 ℃ to perform grafting reaction to obtain a product A;
s2, adding the thermoplastic resin with the formula amount into the product A, and mixing for 5-8min at 40-45 ℃ to obtain a product B;
s3, sequentially adding the antioxidant, the plasticizer and the softener in the formula amount into the product B, and mixing for 10-15min to obtain a product C;
s4, adding a reducing agent and an activating agent into the product C, and mixing and gelling for 25-30min to obtain a product D;
s5, extruding and molding the product D to obtain the tungsten-based radiation protection composite material for additive manufacturing.
Preferably, the product D is subjected to calendaring molding in step S5, i.e. a tungsten-based weight material with high specific gravity and/or a radiation protection material with high shielding efficiency in an extreme environment below 100 ℃.
The invention has the beneficial effects that:
(1) obtaining high specific gravity of 4.23-12.37g/cm3The tungsten-based weight material of (a), can be used for equipment weights, including but not limited to fishing sinkers;
(2) the tungsten-based radiation protection composite material with high specific gravity, high shielding efficiency and high plasticity is obtained, can be directly used for radiation protection in an extreme environment below 100 ℃, has good deformability and can be repeatedly used;
(3) the part printed by the composite material through the SLM has good radiation protection and tungsten alloy comprehensive mechanical property;
(4) the problem of difficult forming and processing of the tungsten-based radiation protection material is solved, and the limitation of complex shape of the tungsten-based radiation protection material is broken through;
(5) the application of the additive manufacturing technology in the field of tungsten-based nuclear power radiation shielding parts is pioneered.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention are further described below.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. 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.
If not specifically stated, the raw materials adopted by the invention are all common commercial products, wherein the particle sizes of the tungsten powder and the tungsten carbide powder are both 1-150 μm; the tungsten oxide is nano-scale tungsten oxide, and the preferable particle size is 100-500 nm.
Example 1 a tungsten-based radiation protective composite for additive manufacturing and method of making the same
A tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials in percentage by weight: 91% of tungsten material, 0.21% of grafting treatment agent, 2% of thermoplastic resin, 0.18% of anti-aging agent, 0.18% of plasticizer, 0.18% of softening agent, 5.7% of reducing agent and 0.55% of activating agent;
the tungsten material is metal tungsten powder, the grafting treatment agent is a silane coupling agent, the thermoplastic resin is butyl rubber, the anti-aging agent is wax, the plasticizer is stearic acid, and the softening agent is white oil; the reducing agent is nickel powder, and the activating agent is sodium chloride.
The preparation method comprises the following steps:
s1, mixing the tungsten material and the grafting treatment agent according to the formula ratio, uniformly stirring, stirring under the protection of inert gas at 60-200 ℃, and carrying out grafting reaction to obtain a product A;
s2, adding the thermoplastic resin with the formula amount into the product A, and mixing for 5-8min at 40-45 ℃ to obtain a product B;
s3, sequentially adding the antioxidant, the plasticizer and the softener in the formula amount into the product B, and mixing for 10-15min to obtain a product C;
s4, adding a reducing agent and an activating agent into the product C, and mixing and gelling for 25-30min to obtain a product D;
s5, extruding and molding the product D to obtain the tungsten-based radiation protection composite material for additive manufacturing or carrying out calendaring molding to obtain the tungsten-based counterweight material with high specific gravity and the radiation protection material with high shielding efficiency in an extreme environment below 100 ℃.
Example 2A tungsten-based radiation protective composite for additive manufacturing and method of making the same
A tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials in percentage by weight: 91% of tungsten material, 0.21% of grafting treatment agent, 2% of thermoplastic resin, 0.18% of anti-aging agent, 0.18% of plasticizer, 0.18% of softening agent, 5.7% of reducing agent and 0.55% of activating agent;
the tungsten material is tungsten carbide powder, the grafting treatment agent is a titanate coupling agent, the thermoplastic resin is nylon 6, the anti-aging agent is an anti-aging agent 264, the plasticizer is stearic acid, and the softener is white oil; the reducing agent is cobalt powder, and the activating agent is sodium fluoride.
The preparation method is the same as that of example 1.
Example 3A tungsten-based radiation protective composite for additive manufacturing and method of making the same
A tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials in percentage by weight: 96% of tungsten material, 0.04% of grafting treatment agent, 2% of thermoplastic resin, 0.02% of anti-aging agent, 0.02% of plasticizer, 0.02% of softener, 1.4% of reducing agent and 0.5% of activating agent;
the tungsten material is tungsten carbide powder, the grafting treatment agent is a titanate coupling agent, the thermoplastic resin is nylon 6, the anti-aging agent is an anti-aging agent 264, the plasticizer is stearic acid, and the softener is white oil; the reducing agent is cobalt powder, and the activating agent is sodium fluoride.
The preparation method is the same as that of example 1.
Example 4A tungsten-based radiation protective composite for additive manufacturing and method of making the same
A tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials in percentage by weight: 70% of tungsten material, 0.40% of grafting treatment agent, 5% of thermoplastic resin, 0.20% of anti-aging agent, 0.20% of plasticizer, 0.20% of softener, 23% of reducing agent and 1% of activating agent;
the tungsten material is tungsten oxide, the grafting treatment agent is a titanate coupling agent, the thermoplastic resin is nylon 6, the anti-aging agent is an anti-aging agent 264, the plasticizer is stearic acid, and the softening agent is white oil; the reducing agent is aluminum powder, and the activating agent is sodium fluoride.
The preparation method is the same as that of example 1.
Example 5A tungsten-based radiation protective composite for additive manufacturing and method of making the same
A tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials in percentage by weight: 84.5% of tungsten material, 0.30% of grafting treatment agent, 2% of thermoplastic resin, 0.40% of anti-aging agent, 0.40% of plasticizer, 0.40% of softening agent, 11.5% of reducing agent and 0.5% of activating agent;
the tungsten material is tungsten oxide, the grafting treatment agent is a carboxylic acid type chelating agent, the thermoplastic resin is nylon 6, the anti-aging agent is an anti-aging agent 4010, the plasticizer is stearic acid, and the softener is white oil; the reducing agent is magnesium powder, and the activating agent is sodium nitrate.
The preparation method is the same as that of example 1.
Example 6A tungsten-based radiation protective composite for additive manufacturing and method of making the same
A tungsten-based radiation protection composite material for additive manufacturing is composed of the following raw materials in percentage by weight: 75% of tungsten material, 0.20% of grafting treatment agent, 6% of thermoplastic resin, 0.70% of anti-aging agent, 0.50% of plasticizer, 0.70% of softening agent, 16% of reducing agent and 0.9% of activating agent;
the tungsten material is tungsten oxide, the grafting treatment agent is a silane coupling agent, the thermoplastic resin is nylon 6, the anti-aging agent is an anti-aging agent D, the plasticizer is stearic acid, and the softening agent is white oil; the reducing agent is iron powder, and the activating agent is sodium chloride.
The preparation method is the same as that of example 1.
Comparative example 1
The comparative example is different from example 1 in that the tungsten material is tungsten powder having a particle size of 100nm, and the plasticizer is phthalate.
Comparative example 2
This comparative example differs from example 3 in that the activator is ammonium chloride and the reducing agent is zinc powder.
Comparative example 3
This comparative example differs from example 3 in that the particle size of the tungsten oxide was 600 nm.
Comparative example 4
This comparative example differs from example 3 in that the particle size of the tungsten oxide was 80 nm.
Comparative example 5
A tungsten/PEEK radiation protective composite wire for 3D printing prepared according to the CN201810868684.5 embodiment.
The theoretical sintered densities of the tungsten-based radiation protective composites prepared in examples 1-6 and comparative examples 1-3 and the Selective Laser Melting (SLM) technique used for additive manufacturing are shown in table 1.
TABLE 1 theoretical sintered density of tungsten-based radiation protection composites and SLM articles
Theoretical sintered theoretical density of SLM parts was calculated from the sintered shrinkage ratio.
As can be seen from the above table, in examples 1 to 3, the low-melting-point metal object is laser-clad in the way of realizing additive printing by SLM, so as to achieve the function of realizing bonding and molding of the low-melting-point clad object, and therefore, the tungsten-based radiation protection composite material prepared in examples 1 to 3 has a high initial density, wherein the theoretical density is 11.87 to 12.37g/cm3However, the point theoretical sintered density of the SLM product is lower and is only 13.48 to 16.86 g/cm3。
Meanwhile, since the metal self-propagating reaction is introduced in the embodiments 4 to 6, the laser provided by the SLM is utilized to excite the intermetallic redox reaction, so as to obtain the high-purity metal tungsten, and the rapid cladding of the metal tungsten is realized to achieve the purpose of additive printing, therefore, although the initial density of the tungsten-based radiation protection composite material prepared in the embodiments 4 to 6 is low, wherein the theoretical density is 4.19 to 4.39 g/cm3However, the SLM product point theoretical sintered density is higher and is 17.65-19.19 g/cm3。
The present invention has been further described with reference to specific embodiments, which are only exemplary and do not limit the scope of the present invention. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (6)
1. A tungsten-based radiation protection composite material for additive manufacturing is characterized by comprising the following raw materials in percentage by weight: 70-96% of tungsten material, 0.01-1% of grafting treatment agent, 2-6% of thermoplastic resin, 0.01-1% of anti-aging agent, 0.01-1% of plasticizer, 0.01-1% of softening agent, 1.4-25% of reducing agent and 0.5-1% of activator;
the thermoplastic resin is at least one of natural rubber, synthetic rubber, reclaimed rubber, nylon and polypropylene;
the plasticizer is at least one of stearic acid, zinc oxide and acrylate copolymer;
the reducing agent is at least one of cobalt powder, nickel powder, magnesium powder, silver powder, aluminum powder and iron powder; the activating agent is at least one of sodium fluoride, sodium chloride, sodium nitrate and sodium sulfite.
2. The tungsten-based radiation protective composite of claim 1 wherein said tungsten material is at least one of tungsten powder, tungsten carbide powder, and tungsten oxide.
3. The tungsten-based radiation protective composite of claim 1, wherein said grafting treatment agent is at least one of a silane coupling agent, a titanate coupling agent, and a carboxylic acid type chelating agent.
4. The tungsten-based radiation protective composite material of claim 1, wherein the antioxidant is at least one of ketoamine, antioxidant D, antioxidant 4010, and antioxidant 264.
5. The tungsten-based radioprotective composite of claim 1, wherein the softening agent is at least one of a pine oil system, a petroleum system, a coal tar system, and a fatty oil system.
6. A method of making the tungsten-based radiation protective composite of any one of claims 1 to 5, comprising the steps of:
s1, mixing the tungsten material and the grafting treatment agent according to the formula ratio, uniformly stirring, and stirring at 60-200 ℃ to perform grafting reaction to obtain a product A;
s2, adding the thermoplastic resin with the formula amount into the product A, and mixing for 5-8min at 40-45 ℃ to obtain a product B;
s3, sequentially adding the antioxidant, the plasticizer and the softener in the formula amount into the product B, and mixing for 10-15min to obtain a product C;
s4, adding a reducing agent and an activating agent into the product C, and mixing and gelling for 25-30min to obtain a product D;
s5, extruding and molding the product D to obtain the tungsten-based radiation protection composite material for additive manufacturing.
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| JP2013144827A (en) * | 2012-01-13 | 2013-07-25 | Advanced Systems Japan Inc | Mechanical alloying material, and insole and radiation protection sheet using the same |
| CN109014174A (en) * | 2018-08-02 | 2018-12-18 | 华南理工大学 | A kind of 3D printing composite material and preparation method of SEBS cladding tungsten |
| CN109251328A (en) * | 2018-08-02 | 2019-01-22 | 华南理工大学 | A kind of tungsten for 3D printing/PEEK radiation protection composite wire and preparation method thereof |
| CN109836710A (en) * | 2019-04-15 | 2019-06-04 | 广州新莱福磁材有限公司 | Super soft X/ gamma-rays protective materials of one kind and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013144827A (en) * | 2012-01-13 | 2013-07-25 | Advanced Systems Japan Inc | Mechanical alloying material, and insole and radiation protection sheet using the same |
| CN109014174A (en) * | 2018-08-02 | 2018-12-18 | 华南理工大学 | A kind of 3D printing composite material and preparation method of SEBS cladding tungsten |
| CN109251328A (en) * | 2018-08-02 | 2019-01-22 | 华南理工大学 | A kind of tungsten for 3D printing/PEEK radiation protection composite wire and preparation method thereof |
| CN109836710A (en) * | 2019-04-15 | 2019-06-04 | 广州新莱福磁材有限公司 | Super soft X/ gamma-rays protective materials of one kind and preparation method thereof |
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