CN108640673B - Wave-absorbing gradient material based on 3D printing technology and preparation method thereof - Google Patents
Wave-absorbing gradient material based on 3D printing technology and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a preparation method of a wave-absorbing gradient material based on a 3D printing technology, and belongs to the field of wave-absorbing coating materials. The wave-absorbing gradient material is of a layered stacked structure and has magnetic conductivity (mu)r) And dielectric constant (. epsilon.)r) The wave-absorbing gradient material is gradually reduced in the thickness direction, the minimum layer is reached at the last layer contacting with air, the wave-absorbing gradient material is composed of a nano absorbent and a polymer, and the nano absorbent is uniformly dispersed in the polymer. The nano absorbent is uniformly dispersed in the polymer, so that the weather resistance of the wave absorbing material is improved on the premise of not influencing the wave absorbing performance; meanwhile, the material with reduced electromagnetic parameter gradient is selected by the impedance matching principle, so that the proportion of electromagnetic waves incident into the material is increased, and the absorption effect of the material on the electromagnetic waves is enhanced.
Description
Technical Field
The invention relates to the field of wave-absorbing coating materials, in particular to a wave-absorbing gradient material based on a 3D printing technology and a preparation method thereof.
Background
The development of science and technology is changing day by day, so that a great deal of advanced electronic products and electrical equipment enter the life, production, national defense, military and commercial application of people, and on one hand, the advanced electronic products and the electrical equipment provide great convenience for the life of people; on the other hand, electronic products and electrical equipment also generate electromagnetic pollution in the using process, thereby causing great threat to physical and psychological health of people. In the military field, with the rapid development of radar technology, the traditional wave-absorbing materials (ferrite, silicon carbide, graphite) and the like cannot realize effective stealth of aircrafts due to the defects of narrow absorption frequency band, high density and the like. Because the wave-absorbing material with the thickness, the lightness, the width and the strength is developed and applied to the military field, the radar detection probability of the aircraft can be improved, and the survival probability of the aircraft in war can be effectively improved. Taking a stealth coating as an example, the characteristics of the coating determine that the construction difficulty is high, and the uniformity of the coating thickness is difficult to control; when the thickness of the coating is large, the coating is easy to crack due to residual air holes generated by volatilization of a large amount of solvent, so that the mechanical property of the invisible coating can hardly meet the actual requirement.
Compared with the traditional process, the 3D printing technology is a novel material processing technology, and is a technology for constructing an object by using bondable materials such as powdered metal or plastic and the like in a layer-by-layer printing mode on the basis of a digital model file. The appearance of the technology enables the composition and the structure of the material to be accurately regulated and controlled on a microscopic scale, so that the possibility of further accurately regulating and controlling the performance of the material is provided. The technology does not need a solvent, can directly print and form on the surface of a target structure, the combination of molecular levels enables the mechanical property between film bases to be higher, and can realize the fine adjustment of electromagnetic parameters in a submicron scale, thereby realizing the wave absorption of a wide frequency band under thinner thickness.
Patent application 201710537669.8 discloses a 3D printing anisotropic microwave absorber and a method for making the same, the microwave absorber is made from magnetic powder with easy-to-plane anisotropy, including rare earth intermetallic compound material with easy-to-plane magnetocrystalline anisotropy. The method has the similar point with the method for preparing the wave-absorbing material, but the wave-absorbing material is a homogeneous wave-absorbing material and has poor impedance matching with free space.
Zhouding et al in article 3D printing technology preparation structure absorbing material and its performance research, apply 3D printing technology to prepare structure absorbing material, choose plastic substrate to add certain amount of absorbent to prepare into mixed powder, prepare the screw and nut structure with SLS (selective laser sintering) mode. However, the material prepared in the article is in direct contact with air, the impedance matching is poor, a large amount of electromagnetic waves are reflected back to the air, and the structure of the screw and the nut is not suitable for large-area coating, so that the practical application is difficult.
In summary, the existing method for preparing the wave-absorbing material by 3D printing of accumulated water still has the problems of narrow absorption band, high density, poor impedance matching between the prepared wave-absorbing material and the free space, and the like, and therefore, a new wave-absorbing gradient material based on the 3D printing technology and a preparation method thereof need to be researched.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a wave-absorbing gradient material based on a 3D printing technology and a preparation method thereof, the invention selects a material with reduced electromagnetic parameter gradient by an impedance matching principle, the prepared gradient wave-absorbing material not only increases the proportion of electromagnetic waves incident into the material, but also enhances the absorption effect of the material on the electromagnetic waves, and meanwhile, the gradient wave-absorbing material prepared by the method has the characteristics of high absorption strength, light weight, thin thickness and the like, and the invention has the advantages of simple process, safety, reliability and convenient operation.
One of the purposes of the invention is to provide a preparation method of a wave-absorbing gradient material based on a 3D printing technology.
The second purpose of the invention is to provide a wave-absorbing gradient material.
The invention also aims to provide a preparation method of the wave-absorbing gradient material based on the 3D printing technology and application of the wave-absorbing gradient material.
In order to achieve the above purpose, the invention specifically discloses the following technical scheme:
the invention discloses a preparation method of a wave-absorbing gradient material based on a 3D printing technology, which comprises the following steps:
(1) mixing a nano absorbent and a polymer, adding the mixture into a dispersing agent, and completely dissolving the polymer in the dispersing agent in a sealed environment to obtain a powder suspension;
(2) drying the powder suspension in the step (1) to obtain powder;
(3) and (3) grinding the powder in the step (2), sintering and molding and 3D printing to obtain the layered stacked wave-absorbing gradient material.
In the step (1), the weight ratio of the nano absorbent, the polymer and the dispersant is (1-5) to (6-8) to (2-9).
In the step (1), the dispersing agent comprises one or more of water, ethanol, acetone, dimethyl ether and ethyl acetate.
In the step (1), the particle size of the absorbent is 1-100 nm.
In the step (1), the nano absorbent is a mixture of dielectric loss powder and magnetic loss powder.
Preferably, the dielectric loss powder comprises one or more of zirconium dioxide, titanium dioxide, zinc oxide, tin oxide, manganese oxide and aluminum oxide.
Preferably, the magnetic loss powder is one or more of polycrystalline iron, ferrite, carbonyl iron, metal powder and iron nitride.
Preferably, the dielectric loss powder and the magnetic loss powder have one or more of a rod shape, a sphere shape, a fiber shape, a flower shape, a dendritic shape, and an irregular shape.
In the step (1), the polymer is one or more of acrylonitrile-butadiene-styrene, polyether ether ketone, polyetherimide and nylon 12.
In the step (1), the dissolution process is carried out at a temperature of 100-150 ℃, and then cooling is carried out by mechanical stirring, preferably, the stirring speed is 100-500 rpm.
Preferably, in the step (2), the powder suspension is filtered through filter paper to form a filter cake, and then the filter cake is dried in a drying oven and then made into powder.
In the step (2), the drying temperature is 80-190 ℃ and the time is 1-10h, and preferably, the drying is carried out in a vacuum environment.
In the step (3), the grinding is carried out in a planetary ball mill, the grinding balls are zirconia balls, the grinding time is 2-10h, the rotating speed of the planetary ball mill is 100-360rpm, and the mass of the grinding balls is 1/3-2/3 of the mass of powder.
In the step (3), the sintering molding and the 3D printing are carried out by adopting a laser sintering system, and the process parameters are as follows: the scanning speed is 1000-4000mm/s, the scanning interval is 0.01-0.5mm, the laser power is 10-80W, and the laser energy density is 0.05-0.15J/mm2The thickness of the single layer is 0.02-0.2 mm.
Secondly, the invention discloses a wave-absorbing gradient material which is of a layered stacked structure and has magnetic conductivity (mu)r) And dielectric constant (. epsilon.)r) The wave-absorbing gradient material is gradually reduced in the thickness direction, the minimum layer is reached at the last layer contacting with air, the wave-absorbing gradient material is composed of a nano absorbent and a polymer, and the nano absorbent is uniformly dispersed in the polymer.
The weight ratio of the nano absorbent, the polymer and the dispersant is (1-5) to (6-8).
The particle size of the absorbent is 1-100 nm.
The nano absorbent is a mixture of dielectric loss powder and magnetic loss powder.
The dielectric loss powder comprises one or more of zirconium dioxide, titanium dioxide, zinc oxide, tin oxide, manganese oxide and aluminum oxide.
Preferably, the dielectric loss powder has one or more of a rod shape, a spherical shape, a fibrous shape, a flower shape, a dendritic shape, and an irregular shape.
Preferably, the magnetic loss powder is one or more of polycrystalline iron, ferrite, carbonyl iron, metal powder and iron nitride.
Preferably, the shape of the magnetic loss powder is one or more of a rod, a sphere, a fiber, a flower, a tree, and an irregularity.
The polymer is one or more of acrylonitrile-butadiene-styrene, polyether ether ketone, polyetherimide and nylon 12.
Finally, the invention also discloses a preparation method of the wave-absorbing material based on the 3D printing technology and application of the wave-absorbing gradient material in electronic products and electrical equipment.
Compared with the prior art, the invention has the beneficial effects that:
(1) the nano absorbent is uniformly dispersed in the polymer, so that the weather resistance of the wave absorbing material is improved on the premise of not influencing the wave absorbing performance; meanwhile, the excellent wave-absorbing performance requires that the wave-absorbing material has large dielectric loss and magnetic loss, and the material with large dielectric loss and magnetic loss has large dielectric constant and magnetic conductivity, so that electromagnetic waves are easy to reflect at the interface of air and the material, the total amount of the electromagnetic waves entering the wave-absorbing material is small, and the total wave-absorbing performance is poor even though the electromagnetic waves are effectively attenuated. The invention selects the material with reduced electromagnetic parameter gradient by the impedance matching principle, so that the electromagnetic wave between the material and the air interface and the internal interface of the material can smoothly pass through, the incidence ratio of the electromagnetic wave into the material is increased, and the absorption effect of the material on the electromagnetic wave is enhanced.
(2) According to the invention, the magnetic conductivity and the dielectric constant of the wave-absorbing material in different thicknesses are adjusted by adjusting the quality of the magnetic loss and dielectric loss material in the polymer, so that the impedance matching of the wave-absorbing material and air is achieved, the reflection loss of the wave-absorbing agent is more than 10dB in the frequency ranges of 2-18GHz and 26-40GHz, and the wave-absorbing agent has good wave-absorbing performance.
(3) The gradient wave-absorbing material prepared by the method has the characteristics of high absorption strength, thin absorption coating, light weight, wide frequency band, strong absorption, good environmental adaptability, good processing performance, economy and environmental protection, can be used for electromagnetic shielding and electronic interference resistance in the fields of electronic products, military equipment and the like, and meanwhile, the method has the advantages of simple process, safety, reliability and convenience in operation.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
Fig. 1 is a schematic structural diagram of a wave-absorbing gradient material prepared based on a 3D printing technology. Wherein the wave-absorbing material is arranged in a layered stack and has magnetic permeability (mu)r) And dielectric constant (. epsilon.)r) Decreasing from bottom to top in the thickness direction.
FIG. 2 is a schematic view of a layered wave-absorbing layer in the wave-absorbing gradient material prepared by the present invention. Wherein 1 represents a magnetic loss material, 2 represents a polymer, and 3 represents a dielectric loss material
Fig. 3 is a reflection loss diagram of the wave-absorbing gradient material prepared in embodiment 1 of the present invention.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. 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 application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As introduced in the background art, the existing method for preparing the wave-absorbing material by the 3D printing technology still has the problems of narrow absorption band, large density, poor impedance matching between the prepared wave-absorbing material and a free space, and the like, so that the invention provides the wave-absorbing gradient material based on the 3D printing technology and the preparation method thereof, and the invention is further described with reference to the accompanying drawings and the specific embodiments.
Example 1
As shown in fig. 1-3, a method for preparing a wave-absorbing gradient material based on a 3D printing technology includes the following steps:
(1) taking 900g of the total amount of raw materials, placing polycrystalline iron with the particle size of 50-100nm, zinc oxide, nylon 12 and ethanol in a stainless steel pressure kettle according to the mass ratio of 1:6:2, sealing the pressure kettle, slowly heating to 100 ℃ to completely dissolve the nylon 12 in the ethanol, and cooling to room temperature under the mechanical stirring of 400rpm to obtain powder suspension;
(2) filtering the powder suspension liquid obtained in the step 1 by using filter paper to obtain a filter cake, and drying the filter cake in a vacuum drying oven at 150 ℃ for 5 hours to obtain powder;
(3) putting the powder obtained in the step (2) into a planetary ball mill, adding zirconia balls with the mass of 2/3 powder, and carrying out ball milling for 5 hours at the rotating speed of 200rpm to obtain coating powder;
(4) sintering, molding and printing the film-coated powder in the step (3) by using a Hanbang laser SLM-2803D printer, wherein the laser sintering process parameters are as follows: the scanning speed is 1000mm/s, the scanning interval is 0.5mm, the laser power is 10W, and the laser energy density is 0.1J/mm2The thickness of a single layer is 0.02 mm;
example 2
A preparation method of a wave-absorbing gradient material based on a 3D printing technology comprises the following steps:
(1) taking 900g of raw materials, placing carbonyl iron with the particle size of 30-90nm, titanium dioxide, acrylonitrile-butadiene-styrene and dimethyl ether in a stainless steel pressure kettle according to the mass ratio of 1:6:2, sealing the pressure kettle, slowly heating to 120 ℃, completely dissolving the acrylonitrile-butadiene-styrene in the dimethyl ether, and cooling to room temperature under the mechanical stirring of 100rpm to obtain powder suspension;
(2) filtering the powder suspension liquid obtained in the step 1 by using filter paper to obtain a filter cake, and drying the filter cake in a vacuum drying oven at the temperature of 80 ℃ for 10 hours to obtain powder;
(3) putting the powder obtained in the step (2) into a planetary ball mill, adding a zirconia ball with the mass of 1/3 powder, and carrying out ball milling for 2 hours at the rotating speed of 360rpm to obtain coating powder;
(4) sintering the coated powder in the step (3) by using a Hanbang laser SLM-2803D printerForming and printing the knot, wherein the process parameters of laser sintering are as follows: the scanning speed is 2000mm/s, the scanning interval is 0.25mm, the laser power is 20W, and the laser energy density is 0.15J/mm2The single-layer thickness is 0.02 mm;
example 3
A preparation method of a wave-absorbing gradient material based on a 3D printing technology comprises the following steps:
(1) taking 1900g of the total amount of raw materials, placing iron nitride, manganese oxide, polyether-ether-ketone and water with the particle size of 70-100nm in a stainless steel pressure kettle according to the mass ratio of 2:8:9, sealing the pressure kettle, slowly heating to 140 ℃, completely dissolving the polyether-ether-ketone in the water, and cooling to room temperature under the mechanical stirring of 500rpm to obtain a powder suspension;
(2) filtering the powder suspension liquid obtained in the step 1 by using filter paper to obtain a filter cake, and drying the filter cake in a vacuum drying oven at 190 ℃ for 1h to obtain powder;
(3) putting the powder obtained in the step (2) into a planetary ball mill, adding zirconia balls with the mass of 1/3 powder, and carrying out ball milling for 10 hours at the rotating speed of 100rpm to obtain coating powder;
(4) sintering, molding and printing the film-coated powder in the step (3) by using a Hanbang laser SLM-2803D printer, wherein the laser sintering process parameters are as follows: the scanning speed is 1000mm/s, the scanning interval is 0.5mm, the laser power is 10W, and the laser energy density is 0.1J/mm2The single-layer thickness is 0.05 mm;
example 4
A preparation method of a wave-absorbing gradient material based on a 3D printing technology comprises the following steps:
(1) taking 500g of the total amount of raw materials, placing ferrite, tin oxide, polyetherimide and ethyl acetate with the particle size of 1-40nm in a stainless steel pressure kettle according to the mass ratio of 5:7:8, sealing the pressure kettle, slowly heating to 150 ℃ to completely dissolve the polyetherimide in the ethyl acetate, and cooling to room temperature under the mechanical stirring of 200rpm to obtain powder suspension;
(2) filtering the powder suspension liquid obtained in the step 1 by using filter paper to obtain a filter cake, and drying the filter cake in a vacuum drying oven at the temperature of 100 ℃ for 6 hours to obtain powder;
(3) putting the powder obtained in the step (2) into a planetary ball mill, adding a zirconia ball with the mass of 1/3 powder, and carrying out ball milling for 8 hours at the rotating speed of 300rpm to obtain coating powder;
(4) sintering, molding and printing the film-coated powder in the step (3) by using a Hanbang laser SLM-2803D printer, wherein the laser sintering process parameters are as follows: the scanning speed is 4000mm/s, the scanning interval is 0.01mm, the laser power is 80W, and the laser energy density is 0.05J/mm2The monolayer thickness was 0.2 mm.
Example 5
A preparation method of a wave-absorbing gradient material based on a 3D printing technology comprises the following steps:
(1) taking 1800g of the total amount of raw materials, placing Fe powder with the particle size of 2-60nm, zirconium dioxide, polyether-ether-ketone and acetone into a stainless steel pressure kettle according to the mass ratio of 3:6:9, sealing the pressure kettle, slowly heating to 100 ℃, completely dissolving the polyether-ether-ketone into the acetone, and cooling to room temperature under the mechanical stirring of 300rpm to obtain a powder suspension;
(2) filtering the powder suspension liquid obtained in the step 1 by using filter paper to obtain a filter cake, and drying the filter cake in a vacuum drying oven at 110 ℃ for 5 hours to obtain powder;
(3) putting the powder obtained in the step (2) into a planetary ball mill, adding zirconia balls with the mass of 2/3 powder, and carrying out ball milling for 5 hours at the rotating speed of 250rpm to obtain coating powder;
(4) sintering, molding and printing the film-coated powder in the step (3) by using a Hanbang laser SLM-2803D printer, wherein the laser sintering process parameters are as follows: the scanning speed is 3000mm/s, the scanning interval is 0.05mm, the laser power is 50W, and the laser energy density is 0.1J/mm2The single-layer thickness is 0.1 mm;
and (3) performance testing:
the performance test of the wave-absorbing gradient material prepared in the embodiment 1 of the invention is carried out, and the result is shown in figure 3, and the wave-absorbing gradient material has reflection loss of more than 10dB in the frequency ranges of 2-18GHz and 26-40GHz and has good wave-absorbing performance. The reason for this can be explained as follows: as shown in the structure of figure 1, the dielectric constant and the magnetic permeability of the material are gradually decreased from bottom to top, and the dielectric constant and the magnetic permeability of the material are almost the same as those of air when reaching the first layer, so that a large amount of electromagnetic waves can be incident into the first layer, the reflection and refraction of the electromagnetic waves among different particles and the reflection and refraction inside the particles can consume a part of energy, when the electromagnetic waves continue to propagate downwards, as the dielectric constant and the magnetic permeability between the two layers are close, the electromagnetic waves which can enter the second layer are still more and repeated, and the wave absorbing performance of the material is obviously improved.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (13)
1. A preparation method of a wave-absorbing gradient material based on a 3D printing technology is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing a nano absorbent and a polymer, adding the mixture into a dispersing agent, and completely dissolving the polymer in the dispersing agent in a sealed environment to obtain a powder suspension;
(2) drying the powder suspension in the step (1) to obtain powder;
(3) grinding the powder in the step (2), sintering and molding and 3D printing to obtain the layered stacked wave-absorbing gradient material;
in the step (1), the nano absorbent is a mixture of dielectric loss powder and magnetic loss powder.
2. The method of claim 1, wherein: in the step (1), the weight ratio of the nano absorbent, the polymer and the dispersant is (1-5) to (6-8) to (2-9);
or, in the step (1), the dispersant comprises one or more of water, ethanol, acetone, dimethyl ether and ethyl acetate;
or, in the step (1), the polymer is one or more of acrylonitrile-butadiene-styrene, polyether ether ketone, polyetherimide and nylon 12.
3. The method of claim 1, wherein: the dielectric loss powder comprises one or more of zirconium dioxide, titanium dioxide, zinc oxide, tin oxide, manganese oxide and aluminum oxide;
or the magnetic loss powder is one or more of polycrystalline iron, ferrite, carbonyl iron, metal powder and iron nitride;
or the shapes of the dielectric loss powder and the magnetic loss powder are one or more of rod-shaped, spherical, fibrous, flower-shaped, dendritic and irregular shapes.
4. The method of claim 1, wherein: in the step (1), the particle size of the absorbent is 1-100 nm;
or, in the step (1), the dissolving process is carried out at the temperature of 100-150 ℃, and then mechanical stirring is adopted for cooling;
or, in the step (2), filtering the powder suspension through filter paper to prepare a filter cake, drying the filter cake in a drying oven, and then preparing the filter cake into powder;
or, in the step (2), the drying temperature is 80-190 ℃ and the time is 1-10 h.
5. The method of claim 1, wherein: in the step (1), the stirring speed is 100-500 rpm.
6. The method of claim 1, wherein: in the step (2), the drying is performed in a vacuum environment.
7. The method of claim 1, wherein: in the step (3), the grinding is carried out in a planetary ball mill, the grinding balls are zirconia balls, the grinding time is 2-10h, the rotating speed of the planetary ball mill is 100-360rpm, and the mass of the grinding balls is 1/3-2/3 of the mass of powder.
8. The process according to claim 1, whereinCharacterized in that: in the step (3), the sintering molding is carried out by adopting a laser sintering system, and the process parameters are as follows: the scanning speed is 1000-4000mm/s, the scanning interval is 0.01-0.5mm, the laser power is 10-80W, and the laser energy density is 0.05-0.15J/mm2The thickness of the single layer is 0.02-0.2 mm.
9. A wave-absorbing gradient material, characterized in that: the wave-absorbing gradient material is of a layered stacked structure, the magnetic conductivity and the dielectric constant of the wave-absorbing gradient material are gradually reduced in the thickness direction, the wave-absorbing gradient material is at the minimum in the last layer contacting with air, the wave-absorbing gradient material is composed of a nano absorbent and a polymer, and the nano absorbent is uniformly dispersed in the polymer.
10. The wave absorbing gradient material of claim 9, wherein: the weight ratio of the nano absorbent to the polymer to the dispersant is (1-5) to (6-8); the particle size of the absorbent is 1-100 nm; or the nano absorbent is a mixture of dielectric loss powder and magnetic loss powder.
11. The wave absorbing gradient material of claim 10, wherein: the polymer is one or more of acrylonitrile-butadiene-styrene, polyether ether ketone, polyetherimide and nylon 12;
or the dielectric loss powder comprises one or more of zirconium dioxide, titanium dioxide, zinc oxide, tin oxide, manganese oxide and aluminum oxide;
or the magnetic loss powder is one or more of polycrystalline iron, ferrite, carbonyl iron, metal powder and iron nitride.
12. The wave absorbing gradient material of claim 11, wherein: the dielectric loss powder and the magnetic loss powder are in one or more of rod-shaped, spherical, fibrous, flower-shaped, dendritic and irregular shapes.
13. Use of a wave absorbing gradient material according to any of claims 9-12 in electronic and electrical devices.
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