Nano powder material for 3D printing and preparation method thereof
Technical Field
The invention belongs to the technical field of materials for rapid prototyping, and particularly relates to a nano powder material for 3D printing and a preparation method thereof.
Background
Three-dimensional printing (3D for short) is a rapid prototyping technology, which can divide three-dimensional model data designed by a computer into lamellar model data, and build up and shape specific raw materials layer by layer until the whole entity is constructed. The 3D forming method has the advantages of low cost, no pollution in the working process, high forming speed and the like.
The rapid development of science and technology, the rapid forming technology is widely applied to various fields of life, the materials for 3D printing at present are all plastic materials, metal materials or ceramic-based materials, the cost is high, the comprehensive popularization of 3D printing is greatly limited, thin-wall parts are not easy to form due to the large particle size of 3D rapid forming material powder, the forming precision of small parts is not high enough, and the surface has obvious roughness.
Chinese patent CN104291338A discloses a preparation method of a three-D printing rapid prototyping nano silicon carbide material, which is characterized by comprising the following steps: (1) pretreatment of nano silicon carbide: grinding 5-15% of 3-aminopropyltriethoxysilane and 85-95% of nano silicon carbide at room temperature for 2-6 h to obtain pretreated nano silicon carbide; (2) preparing a rapidly molded nano silicon carbide material: carrying out ultrasonic reaction on 60-75% of absolute ethanol and 20-35% of pretreated nano silicon carbide for 4-6h in an ice bath, adding 2-10% of diphenol propane glycidyl ether, stirring and mixing uniformly, reacting for 8-14 h at a constant temperature of 50 +/-3 ℃, and carrying out spray drying to obtain the rapidly-formed nano silicon carbide material. The material is directly molded at the temperature of 153-159 ℃ and the pressure of 1-10 MPa, and has the advantages of simple preparation process, easily controlled conditions, low production cost and easy industrial production.
Chinese patent CN104310948A discloses a preparation method of a three-D printing rapid prototyping inorganic powder material, which is characterized by comprising the following steps: in a grinding machine, adding vinyltriethoxysilane according to mass percentage: 8-22%, adding inorganic powder materials: 78-92%, starting a grinder to rotate at a speed of 200 rpm, and grinding for 4-6h at room temperature to obtain a pretreated inorganic powder material; then adding the pretreated inorganic powder material into a grinding machine according to the mass percentage concentration: 85% -96%, adding EVA hot melt adhesive powder: 4% -15%, starting a grinder to rotate at a speed of 200 rpm, and grinding at room temperature for 4-6h to obtain the three-D printing rapid prototyping inorganic powder material. The preparation method has the advantages of simple preparation process, easily controlled conditions, low production cost and easy industrial production. The material can be directly molded without spraying a binder under the conditions of heating at 140-180 ℃ and pressure within the range of 2-6 MPa, and the molding operation is simple.
Therefore, aiming at the problems, the invention provides the nano powder material for 3D printing, which has the characteristics of rapid forming, stable structure, low production cost and long service life.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provide a nano powder material for 3D printing, and solve the problems of limited application, complex preparation process and high material cost of the existing powder material for D printing.
In order to solve the technical problems, the invention adopts the following technical scheme:
a nano powder material for 3D printing is composed of the following raw materials in parts by weight: 30 to 45 portions of nano carbon fiber, 10 to 20 portions of nano glass fiber, 20 to 40 portions of nano magnesium oxide, 4 to 6 portions of surface reinforcing agent, 0.8 to 1.6 portions of antioxidant and 0.6 to 0.8 portion of toughening agent; the surface reinforcing agent is a combination of boron oxide, gypsum and a silane coupling agent; the mass ratio of the boron oxide to the gypsum to the silane coupling agent is 2: 2: 3.
further, the nano powder material for 3D printing is composed of the following raw materials in parts by weight: 40 parts of carbon nanofiber, 16 parts of glass nanofiber, 32 parts of nano magnesium oxide, 5 parts of surface reinforcing agent, 1.2 parts of antioxidant and 0.7 part of toughening agent.
Further, the antioxidant is one or a combination of β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid octadecyl ester, 1, 3-tri (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, tri [2, 4-di-tert-butylphenyl ] phosphite, dilauryl thiodipropionate and triphenyl nitrite.
Furthermore, the toughening agent is one or a combination of styrene-butadiene thermoplastic elastomer, methyl methacrylate-butadiene-styrene terpolymer, acrylonitrile-butadiene-styrene copolymer, chlorinated polyethylene and ethylene-vinyl acetate copolymer.
The main components have the following functions:
the surface reinforcing agent can effectively improve the surface structures of the carbon nanofibers, the glass nanofibers and the magnesium oxide nanoparticles, enhance the compatibility among the raw materials, better combine the toughening agent and the antioxidant, and avoid the prepared nano powder material for 3D printing from layering and falling off in the printing process; the antioxidant enhances the fusion force among the raw materials, and simultaneously enables the nano powder material for 3D printing to be easy to form in the printing process, is antioxidant and has long service life; the toughening agent is added to improve the tensile, compression and impact resistance of the nano powder material for 3D printing, so that the nano powder material is convenient to form, and meanwhile, the nano powder material for 3D printing has a wider application range and longer service life.
According to another aspect of the present invention, there is provided a method for preparing the nano powder material for 3D printing, including the steps of:
s10, preparing the surface reinforcing agent in parts by weight into a solution with the mass percent of 8% -10% by using ethanol, adding the solution into a grinding machine, adding the nano glass fiber and the nano carbon fiber in parts by weight, and grinding the mixture for 1-4 hours by using the grinding machine at the temperature of 35-40 ℃ to obtain a component A;
s20, adding the nano magnesium oxide in the weight part into the component A obtained in the S10, grinding for 2-6 h at the temperature of 30-35 ℃, filtering and drying for 4h at the normal pressure and the temperature of 115-120 ℃ to obtain a component B;
and S30, crushing the component B obtained in the step S20, sieving the crushed component B with a 60-100-mesh sieve, adding the antioxidant and the flexibilizer in parts by weight, oscillating the mixture for 30-60 min, carrying out ultrasonic treatment for 2-3 h at the temperature of 65-75 ℃, carrying out hot melting plasticization on the mixture by a double-screw extruder, granulating the mixture by a granulator, cooling the obtained granules, and crushing the granules to obtain the 3D printing nano powder material.
Further, in S10, the rotation speed of the grinder is 600 r/min-1000 r/min.
Further, in S20, the rotating speed of the grinder is 400 r/min-800 r/min.
Further, in S30, the hot melt plasticizing temperature is 230 ℃ to 255 ℃.
Further, in S30, the temperature of the pelletizer is 150 ℃ to 160 ℃.
Furthermore, in S30, the particle size of the nano powder material for 3D printing is 30nm to 40 nm.
The invention has the advantages and beneficial effects that:
1. according to the nano powder material for 3D printing disclosed by the invention, the basic performance of the nano powder material for 3D printing is enhanced by adding the nano glass fiber and the nano carbon fiber, so that the nano powder material can be rapidly formed without delaminating in the printing process, and meanwhile, the mechanical strength and the light induction strength of the nano powder material can be enhanced by the nano glass fiber, so that a product formed by 3D printing has excellent luster and aesthetic feeling; the nano magnesium oxide is added to enhance the compression resistance and impact resistance of the nano powder material for 3D printing and keep the stable structure of the 3D printing molded product; by adding other flexibilizers and antioxidants, all raw materials interact with each other, the internal binding force of the 3D printing nano material is enhanced, the performance of the 3D printing nano powder material is improved, the product quality is improved together, and the application is wider;
2. the nano powder material for 3D printing disclosed by the invention can reduce the production cost, can avoid the problem that the application range of the nano powder material is limited due to price factors in the current market, and meanwhile, the nano split material for 3D printing disclosed by the invention has good wear resistance and long service life;
3. the nano powder material for 3D printing disclosed by the invention is strong in stereoscopic impression, is applied to the 3D printing process, reduces the cost, improves the aesthetic feeling and the mechanical strength of the product, and is very suitable for wide popularization.
4. The invention combines the modern advanced technology, the preparation method is simple, the processing cost is low, and the prepared nano powder material for 3D printing has good quality and is convenient to use.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
Example 1
Nano powder material for 3D printing
The raw materials and the ingredients comprise: (unit: g)
The nano powder material for 3D printing is composed of the following raw materials in parts by weight: 300g of carbon nanofiber, 100g of glass nanofiber, 200g of nano magnesium oxide, 40g of surface reinforcing agent, 8g of antioxidant and 6g of toughening agent; the surface reinforcing agent is a combination of boron oxide, gypsum and a silane coupling agent; the mass ratio of the boron oxide to the gypsum to the silane coupling agent is 2: 2: 3.
the preparation method comprises the following steps:
s10, preparing the surface reinforcing agent in parts by weight into an ethanol solution with the mass percent of 8%, adding the ethanol solution into a grinding machine, adding the nano glass fiber and the nano carbon fiber in parts by weight, and grinding the grinding machine for 1h at the temperature of 35 ℃ and the rotating speed of 600r/min to obtain a component A;
s20, adding the nano magnesium oxide in parts by weight into the component A obtained in the S10, grinding for 2 hours at the temperature of 30 ℃ and the rotating speed of a grinder of 400r/min, filtering, and drying for 4 hours at the normal pressure and the temperature of 115 ℃ to obtain a component B;
and S30, crushing the component B obtained in the step S20, sieving the crushed component B with a 60-mesh sieve, adding the antioxidant and the flexibilizer in parts by weight, oscillating the obtained mixture for 30min, carrying out ultrasonic treatment for 2h at the temperature of 65 ℃, carrying out hot melting plasticization on the obtained product by a double-screw extruder at the temperature of 230 ℃, carrying out granulation on the obtained product by a granulator at the temperature of 150 ℃, and crushing the obtained granules to obtain the 3D printing nano powder material.
In the above operation, the particle size of the nano powder material for 3D printing is 30 nm.
Example 2
Nano powder material for 3D printing
The raw materials and the ingredients comprise: (unit: g)
The nano powder material for 3D printing is composed of the following raw materials in parts by weight: 450g of carbon nanofiber, 200g of glass nanofiber, 400g of nano magnesium oxide, 60g of surface reinforcing agent, 16g of antioxidant and 8g of toughening agent; the surface reinforcing agent is a combination of boron oxide, gypsum and a silane coupling agent; the mass ratio of the boron oxide to the gypsum to the silane coupling agent is 2: 2: 3.
the preparation method comprises the following steps:
s10, preparing the surface reinforcing agent in parts by weight into a solution with the mass percentage of 10% by using ethanol, adding the solution into a grinding machine, adding the nano glass fiber and the nano carbon fiber in parts by weight, and grinding the grinding machine for 4 hours at the temperature of 40 ℃ and the rotating speed of 1000r/min to obtain a component A;
s20, adding the nano magnesium oxide in parts by weight into the component A obtained in the S10, grinding for 6 hours at the temperature of 35 ℃ and the rotation speed of 800r/min, filtering, and drying for 4 hours at the normal pressure and the temperature of 120 ℃ to obtain a component B;
and S30, crushing the component B obtained in the step S20, sieving the crushed component B with a 100-mesh sieve, adding the antioxidant and the flexibilizer in parts by weight, oscillating for 60min, carrying out ultrasonic treatment for 3h at the temperature of 75 ℃, carrying out hot melting plasticization on the obtained product by a double-screw extruder at the temperature of 255 ℃, carrying out granulation by a granulator at the temperature of 160 ℃, cooling the obtained granules, and crushing the granules to obtain the 3D printing nano powder material.
In the above operation, the particle size of the nano powder material for 3D printing is 40 nm.
Example 3
Nano powder material for 3D printing
The raw materials and the ingredients comprise: (unit: g)
The nano powder material for 3D printing is composed of the following raw materials in parts by weight: 350g of carbon nanofiber, 120g of glass nanofiber, 240g of nano magnesium oxide, 46g of surface reinforcing agent, 10g of antioxidant and 6.8g of toughening agent; the surface reinforcing agent is a combination of boron oxide, gypsum and a silane coupling agent; the mass ratio of the boron oxide to the gypsum to the silane coupling agent is 2: 2: 3.
the preparation method comprises the following steps:
s10, preparing the surface reinforcing agent in parts by weight into a solution with the mass percent of 8% by using ethanol, adding the solution into a grinding machine, adding the nano glass fiber and the nano carbon fiber in parts by weight, and grinding the grinding machine for 2 hours at the temperature of 38 ℃ and the rotating speed of 700r/min to obtain a component A;
s20, adding the nano magnesium oxide in parts by weight into the component A obtained in the S10, grinding for 3 hours at the temperature of 32 ℃ and the rotation speed of 500r/min, filtering, and drying for 4 hours at the normal pressure and the temperature of 116 ℃ to obtain a component B;
and S30, crushing the component B obtained in the step S20, sieving the crushed component B with a 80-mesh sieve, adding the antioxidant and the flexibilizer in parts by weight, oscillating for 40min, carrying out ultrasonic treatment for 2h at the temperature of 65 ℃, carrying out hot melting plasticization on the component B at the temperature of 235 ℃ by using a double-screw extruder, granulating the component B at the temperature of 152 ℃ by using a granulator, cooling the obtained granules, and crushing the granules to obtain the 3D printing nano powder material.
In the above operation, the particle size of the nano powder material for 3D printing is 40 nm.
Example 4
Nano powder material for 3D printing
The raw materials and the ingredients comprise: (unit: g)
The nano powder material for 3D printing is composed of the following raw materials in parts by weight: 400g of carbon nanofiber, 180g of glass nanofiber, 360g of nano magnesium oxide, 560g of surface reinforcing agent, 14g of antioxidant and 7.8g of toughening agent; the surface reinforcing agent is a combination of boron oxide, gypsum and a silane coupling agent; the mass ratio of the boron oxide to the gypsum to the silane coupling agent is 2: 2: 3.
the preparation method comprises the following steps:
s10, preparing the surface reinforcing agent in parts by weight into a solution with the mass percentage of 10% by using ethanol, adding the solution into a grinding machine, adding the nano glass fiber and the nano carbon fiber in parts by weight, and grinding the grinding machine for 3 hours at the temperature of 38 ℃ and the rotating speed of 900r/min to obtain a component A;
s20, adding the nano magnesium oxide in parts by weight into the component A obtained in the S10, grinding for 5 hours at the temperature of 34 ℃ and the rotation speed of 700r/min, filtering, and drying for 4 hours at the normal pressure and the temperature of 120 ℃ to obtain a component B;
and S30, crushing the component B obtained in the step S20, sieving the crushed component B with a 100-mesh sieve, adding the antioxidant and the flexibilizer in parts by weight, oscillating for 50min, carrying out ultrasonic treatment for 3h at the temperature of 72 ℃, carrying out hot melting plasticization on the obtained product by a double-screw extruder at the temperature of 245 ℃, carrying out granulation by a granulator at the temperature of 158 ℃, cooling the obtained granules, and crushing the granules to obtain the 3D printing nano powder material.
In the above operation, the particle size of the nano powder material for 3D printing is 30 nm.
Example 5
Nano powder material for 3D printing
The raw materials and the ingredients comprise: (unit: g)
The nano powder material for 3D printing is composed of the following raw materials in parts by weight: 400g of carbon nanofiber, 160g of glass nanofiber, 320g of nano magnesium oxide, 50g of surface reinforcing agent, 12g of antioxidant and 7g of toughening agent; the surface reinforcing agent is a combination of boron oxide, gypsum and a silane coupling agent; the mass ratio of the boron oxide to the gypsum to the silane coupling agent is 2: 2: 3.
the preparation method comprises the following steps:
s10, preparing the surface reinforcing agent in parts by weight into a 9% solution by mass percent with ethanol, adding the solution into a grinder, adding the nano glass fiber and the nano carbon fiber in parts by weight, and grinding the grinder for 2.4 hours at the temperature of 35 ℃ and the rotating speed of 800r/min to obtain a component A;
s20, adding the nano magnesium oxide in parts by weight into the component A obtained in the S10, grinding for 4 hours at the temperature of 35 ℃ and the rotation speed of 600r/min, filtering, and drying for 4 hours at the normal pressure and the temperature of 120 ℃ to obtain a component B;
and S30, crushing the component B obtained in the step S20, sieving the crushed component B with a 80-mesh sieve, adding the antioxidant and the flexibilizer in parts by weight, oscillating for 45min, carrying out ultrasonic treatment for 2.5h at the temperature of 70 ℃, carrying out hot melting plasticization on the component B at the temperature of 240 ℃ by using a double-screw extruder, carrying out granulation on the component B at the temperature of 155 ℃ by using a granulator, cooling the obtained granules, and crushing the granules to obtain the 3D printing nano powder material.
In the above operation, the particle size of the nano powder material for 3D printing is 40 nm.
Examples of the experiments
The 3D printing nano powder material prepared by the above embodiments 1-5 is used for the research of the basic performance of the 3D printing nano powder material, and further confirms the function of the 3D printing nano powder material:
test 1: the basic performance of the 3D printing nano powder material prepared in examples 1 to 5 was tested, and the test results are shown in table 1:
table 1 results of basic performance test of nano powder material for printing in examples 1-53D
As can be seen from Table 1, the pH value of the 3D printing nano powder material prepared in examples 1-5 is neutral, and the wear-resistant strength, impact strength, permeability coefficient, elongation at break and anti-seismic ductility coefficient are stable, so that the nano powder material is suitable for wide application.
In addition, the nano powder material for 3D printing provided by the invention does not delaminate in the using process, has a stable structure, is glossy and attractive, and has a long service life.
The above description is only a preferred embodiment and an experimental example of the present invention, and is not intended to limit the present invention, and it is obvious to those skilled in the art that various modifications and variations can be made in the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.