CN113186481A - Preparation method of wave-absorbing stealth composite coating - Google Patents
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
- C23C4/129—Flame spraying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/00—Amorphous alloys
- C22C45/02—Amorphous alloys with iron as the major constituent
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/02—Pretreatment of the material to be coated, e.g. for coating on selected surface areas
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
- C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
- C23C4/06—Metallic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0824—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with a specific atomising fluid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0848—Melting process before atomisation
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Abstract
The invention relates to a preparation method of a wave-absorbing stealth composite coating, which comprises the following steps: according to Fe-based amorphous alloy Fe85Si4Cu3B6Nb2Weighing Fe, Si, Cu, B and Nb raw materials according to mass fraction percentage; the weighed raw materials are sequentially placed into a vacuum melting furnace according to the sequence of high melting point and low melting point, argon is used as shielding gas, then the temperature is raised to completely melt the raw materials, an iron-based amorphous alloy mother ingot is obtained by cooling, and repeated melting is carried out to ensure that the components of the iron-based amorphous alloy mother ingot are uniform; pretreating and making into small blocks; using the small blockPreparing iron-based amorphous alloy micro powder by an air atomization method; preparing iron-based amorphous/graphene composite powder; preheating; and spraying the obtained iron-based amorphous/graphene composite powder on a substrate by using a supersonic flame spraying method to obtain the wave-absorbing stealth composite coating.
Description
Technical Field
The invention belongs to the technical field of wave-absorbing materials, and particularly relates to a wave-absorbing stealth composite coating.
Background
The wave-absorbing material can be used on military equipment, such as military equipment of military aircrafts, submarines and the like, so that the survival probability and the operational capacity of the weapon equipment in war are improved; the method can also be applied to industrial equipment, and can be used for improving the anti-interference capability of electronic equipment, enhancing the security and confidentiality and realizing the security protection. Research on the wave-absorbing material mainly focuses on two aspects, on one hand, the high-performance requirements such as high absorption rate, light weight, high temperature resistance and the like are pursued, and the advanced technological requirements such as radar reconnaissance resistance in military are met; on the other hand, the method aims to reduce the cost and meet the requirements of large-scale production and use.
The iron element has the advantages of abundant reserves and easy acquisition in nature, and the iron-based amorphous alloy material has a unique structure with long-range disorder and short-range order, so that the iron-based amorphous alloy material has excellent soft magnetic performance and can be used as a novel wave-absorbing material. However, when a single iron-based amorphous alloy is used as a wave-absorbing material, the impedance matching characteristic of the alloy is unbalanced, and the defects of unsatisfactory wave-absorbing performance, large thickness, narrow wave-absorbing band width and the like still exist.
Disclosure of Invention
The invention provides a preparation method of a novel wave-absorbing stealth composite coating, which is characterized in that Fe, Nb, Si, Cu and B are taken as the basis, a small amount of graphene powder is added, and Fe is prepared by a supersonic flame spraying technology85Si4Cu3B6Nb2Wave-absorbing stealth composite coating. The technical scheme adopted by the invention is as follows:
a preparation method of the wave-absorbing stealth composite coating comprises the following steps:
(1) according to Fe-based amorphous alloy Fe85Si4Cu3B6Nb2Weighing Fe, Si, Cu, B and Nb raw materials according to mass fraction percentage;
(2) the weighed raw materials are sequentially placed into a vacuum melting furnace according to the sequence of high melting point and low melting point, argon is used as shielding gas, then the temperature is raised to completely melt the raw materials, the raw materials are cooled to obtain an iron-based amorphous alloy mother ingot, and the melting is repeated for more than 3 times to ensure that the components of the iron-based amorphous alloy mother ingot are uniform.
(3) Carrying out pretreatment including polishing to remove surface oxide skin and ultrasonic cleaning on the prepared iron-based amorphous alloy master ingot, and preparing the iron-based amorphous alloy master ingot into a small block;
(4) preparing the prepared small blocks into iron-based amorphous alloy micro powder by using a vacuum atomization method;
(5) mixing the iron-based amorphous alloy micro powder prepared in the step (4) with graphene micro powder according to the ratio of (85-95): (5-15) fully mixing the components in percentage by mass to obtain iron-based amorphous/graphene composite powder; the method comprises the following steps:
(6) the method is characterized in that the method in the step (5) is as follows:
1) mixing iron-based amorphous alloy micro powder and graphene micro powder, and adding the mixture into a container containing absolute ethyl alcohol;
2) fully and uniformly mixing the iron-based amorphous alloy micro powder and the graphene micro powder through mechanical stirring and ultrasonic oscillation;
3) and (3) drying the mixture in vacuum to volatilize the absolute ethyl alcohol, thereby obtaining the iron-based amorphous/graphene composite powder.
(7) Cleaning and cleaning the surface of a substrate needing to be coated, sandblasting and roughening the surface, and preheating the surface to ensure that the temperature of the substrate reaches over 180 ℃;
(8) and (4) spraying the obtained iron-based amorphous/graphene composite powder on the substrate treated in the step (7) by using a supersonic flame spraying method, and finally obtaining the wave-absorbing stealth composite coating.
Further, when the mass fraction of the graphene is 10%, the thickness of the coating is 3 mm.
The substrate is a steel plate substrate.
For the iron-based amorphous alloy, the amorphous forming capability of the alloy is influenced by excessively high iron content, and the saturation induction strength Bs is lower than 1.7T due to excessively low iron content, so that the iron-based amorphous alloy cannot be suitable for high-power products. The invention adds small amount of non-metallic elements of Si and B by micro-alloying, so that the alloy has a larger annealing interval, Tx is 109. The alloy has a higher glass transition temperature Tg of 753K, and the addition of Si effectively inhibits the precipitation of FeB secondary phase. The trace addition of Nb can not only improve the amorphous forming capability of the alloy, but also hinder the formation of crystal grains, and improve the thermal stability of the alloy and the corrosion resistance of the prepared composite coating. The iron-based amorphous alloy has high amorphous forming ability and stability by adjusting the component proportion of the iron-based amorphous alloy and enabling atoms to have a large degree of atom mismatching. The saturated magnetic induction strength Bs of the wave-absorbing stealth composite coating prepared by the method provided by the invention is in a range of 1.7-1.9T, the yield strength is 2.67GPa, the breaking strength is 2.9GPa, and the Vickers hardness is 870 Hv. According to the invention, a small amount of graphene is added into the iron-based amorphous alloy, so that the wave absorbing performance of the composite coating is improved.
Drawings
FIG. 1 is an iron-based amorphous alloy powder prepared by the method of the present invention and graphene powder used;
FIG. 2 is a wave-absorbing stealth composite coating prepared by the method of the present invention;
FIG. 3 is a reflection attenuation curve of the wave-absorbing stealth composite coating prepared by the method of the invention under different composite proportions.
Detailed Description
The method for preparing the composite material by adding the graphene into the iron-based amorphous alloy improves the wave absorbing property of the alloy, and provides the preparation method for preparing the wave absorbing stealth composite coating with small thickness, low density, wide absorption frequency band and strong wave absorbing capacity.
In order to make the technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings.
The first step is as follows: according to Fe85Si4Cu3B6Nb2The raw materials of Fe, Si, Cu, B and Nb are weighed according to the mass fraction percentage, the purity of the used raw materials is more than 99.99 percent, and the raw materials are purchased from the new material science and technology company of Mitsui in Beijing. The existing wave-absorbing material is mainly made of iron-cobalt-based alloy, while the iron-based alloy also contains cobalt and nickel metal elements with larger proportion, so that the problems of high cost, low single alloy absorptivity and the like exist85Si4Cu3B6Nb2The alloy is prepared into an amorphous material, so that the wave-absorbing and corrosion-resisting properties of the material can be improved, the cost is reduced, and the wave-absorbing property of the material is improved by adding a certain amount of graphene.
The second step is that: sequentially putting the raw materials into a vacuum arc melting furnace according to the sequence of high melting point and low melting point, heating to completely melt the raw materials, and cooling to obtain the iron-based amorphous alloy master ingot. The vacuum degree in the furnace in the smelting process is ensured to reach 6 multiplied by 10-3And Pa, filling argon as a protective gas to prevent the smelting process from being oxidized. The smelting is repeated for 3-4 times to ensure that the components of the iron-based amorphous alloy mother ingot are uniform.
The second step is that: the iron-based amorphous alloy mother ingot alloy is prepared by a vacuum aerosol furnace to obtain iron-based amorphous alloy powder, and the iron-based amorphous alloy powder with the particle size of 30-53 mu m is obtained by screening the particle size. Argon is used as protective atmosphere when the vacuum atomization furnace is used for preparing the iron-based amorphous alloy powder, and the gas atomization pressure is 3 MPa.
The third step: iron-based amorphous alloy powder and graphene powder are respectively mixed according to the weight ratio of 85: 15. 90: 10. 95: 5, adding the mixture into absolute ethyl alcohol, mechanically stirring for 30min, and ultrasonically oscillating for 30min to fully and uniformly mix the iron-based amorphous alloy powder and the graphene powder. As shown in fig. 1, the iron-based amorphous alloy powder is on the left side, and the graphene powder is on the right side.
The fourth step: and after mechanical stirring and ultrasonic oscillation are carried out in the third step, the mixture is dried for 2 hours in vacuum at the temperature of 90 ℃ to obtain the iron-based amorphous/graphene composite powder.
The fifth step: cleaning and cleaning the surface of the steel substrate, sandblasting and coarsening and preheating. The method comprises the following steps: sequentially polishing by using 200, 320 and 800-mesh abrasive paper, and then cleaning by using gasoline and alcohol to remove stains; using Al2O3Carrying out sand blasting coarsening treatment on the particles, wherein the sand blasting coarsening treatment is carried out within two hours before spraying; and (3) carrying out quick-sweeping preheating treatment on the surface of the substrate by using an HVOF supersonic flame spray gun to enable the temperature of the substrate to reach about 200 ℃.
And a sixth step: spraying the obtained iron-based amorphous/graphene composite powder on the steel substrate treated in the step S6 by using a supersonic flame spraying technology, wherein the spraying process parameters are as follows: the flow rate of kerosene is 24L/h, the flow rate of oxygen is 32L/h, the powder feeding speed is 30g/min, the powder feeding pressure is 4.8MPa, and the spraying distance is 360mm, thus finally obtaining the wave-absorbing stealth composite coating. As shown in fig. 2, the prepared wave-absorbing stealth composite coating is provided. The reflection attenuation curves of the obtained wave-absorbing stealth composite coating under different composite proportions are shown in figure 3, when graphene is not added, the absorption peak extreme value of the iron-based amorphous alloy is-13.1 dB, when a proper amount of graphene is added, the absorption peak extreme value is obviously improved, and the reflection attenuation curves of the obtained wave-absorbing stealth composite coating are as follows, wherein the reflection attenuation curves of the obtained wave-absorbing stealth composite coating under different composite proportions are as shown in figure 3, when graphene is not added, the absorption peak extreme value of the iron-based amorphous alloy is-13.1 dB, and when a proper amount of graphene is added, the absorption peak extreme value of the obtained wave-absorbing stealth composite coating is as follows, the reflection attenuation curves of the obtained wave-absorbing stealth composite coating are as shown in the specification, wherein the reflection attenuation curve of the iron-based amorphous alloy and the graphene are as follows: 10, the absorption peak extreme value is-27.2 dB, the corresponding absorption frequency is 12GHz, and the wave-absorbing capacity is maximum. Meanwhile, when graphene is not added, the real part epsilon 'of the complex dielectric constant of the iron-based amorphous alloy is 6.1, and the imaginary part epsilon' is 0.47. And the ratio of the iron-based amorphous alloy to the graphene is 90: when the mass fraction of 10 is compounded, the real part epsilon 'of the complex dielectric constant is 23, the imaginary part epsilon' is 8.9, the dielectric constant is obviously increased, and the electromagnetic wave absorption capacity of the material is obviously improved.
Claims (3)
1. A preparation method of the wave-absorbing stealth composite coating comprises the following steps:
(1) according to Fe-based amorphous alloy Fe85Si4Cu3B6Nb2Weighing Fe, Si, Cu, B and Nb raw materials according to mass fraction percentage;
(2) the weighed raw materials are sequentially placed into a vacuum melting furnace according to the sequence of high melting point and low melting point, argon is used as shielding gas, then the temperature is raised to completely melt the raw materials, the raw materials are cooled to obtain an iron-based amorphous alloy mother ingot, and the melting is repeated for more than 3 times to ensure that the components of the iron-based amorphous alloy mother ingot are uniform.
(3) Carrying out pretreatment including polishing to remove surface oxide skin and ultrasonic cleaning on the prepared iron-based amorphous alloy master ingot, and preparing the iron-based amorphous alloy master ingot into a small block;
(4) preparing the prepared small blocks into iron-based amorphous alloy micro powder by using a vacuum atomization method;
(5) mixing the iron-based amorphous alloy micro powder prepared in the step (4) with graphene micro powder according to the ratio of (85-95): (5-15) fully mixing the components in percentage by mass to obtain iron-based amorphous/graphene composite powder; the method comprises the following steps:
(6) the method is characterized in that the method in the step (5) is as follows:
1) mixing iron-based amorphous alloy micro powder and graphene micro powder, and adding the mixture into a container containing absolute ethyl alcohol;
2) fully and uniformly mixing the iron-based amorphous alloy micro powder and the graphene micro powder through mechanical stirring and ultrasonic oscillation;
3) drying the mixture in vacuum to volatilize the absolute ethyl alcohol, and obtaining iron-based amorphous/graphene composite powder;
(7) cleaning and cleaning the surface of a substrate needing to be coated, sandblasting and roughening the surface, and preheating the surface to ensure that the temperature of the substrate reaches over 180 ℃;
(8) and (4) spraying the obtained iron-based amorphous/graphene composite powder on the substrate treated in the step (7) by using a supersonic flame spraying method, and finally obtaining the wave-absorbing stealth composite coating.
2. The method for preparing the wave-absorbing stealth composite coating according to claim 1, characterized in that the coating thickness is 3mm when the graphene mass fraction is 10%.
3. The method for preparing the wave-absorbing stealth composite coating according to claim 1, characterized in that the substrate is a steel plate substrate.
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| CN114045435A (en) * | 2021-11-11 | 2022-02-15 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114045435A (en) * | 2021-11-11 | 2022-02-15 | 泉州天智合金材料科技有限公司 | Iron-based amorphous nanocrystalline wave-absorbing material and preparation method thereof |
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