CN111944181A - Method for reducing infrared emissivity of polyimide resin matrix composite material - Google Patents
Method for reducing infrared emissivity of polyimide resin matrix composite material Download PDFInfo
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- CN111944181A CN111944181A CN202010654377.4A CN202010654377A CN111944181A CN 111944181 A CN111944181 A CN 111944181A CN 202010654377 A CN202010654377 A CN 202010654377A CN 111944181 A CN111944181 A CN 111944181A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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Abstract
The invention provides a method for reducing the infrared emissivity of a polyimide resin matrix composite material, which comprises the steps of etching the surface of the polyimide resin matrix composite material by using a strong alkaline solution, immersing the polyimide resin matrix composite material subjected to surface etching into a silver nitrate solution for ion exchange, and then putting the polyimide resin matrix composite material into an oven for heat treatment to finally obtain the polyimide resin matrix composite material with low infrared emissivity. The method for reducing the infrared emissivity of the polyimide resin matrix composite material provided by the invention is simple in process and easy to operate.
Description
Technical Field
The invention discloses a method for reducing the infrared emissivity of a polyimide resin matrix composite material, and belongs to the technical field of infrared stealth.
Technical Field
The infrared detection technology is one of the main methods for detecting military aircrafts at present, and an infrared detection system mainly finds a target by receiving thermal infrared radiation with wave bands of 3-5 microns and 8-14 microns. The high-temperature-resistant polyimide resin-based composite material has the characteristics of high temperature resistance, light weight, high strength and corrosion resistance, is widely applied to military aircrafts, is mainly applied to high-temperature areas of the aircrafts, and has high infrared emissivity. Therefore, in order to improve the concealment and the penetration resistance of military aircraft, it is necessary to reduce the infrared emissivity of the polyimide resin-based composite material.
The prior infrared stealth technology mainly covers a layer of infrared stealth material coating on the surface of a material, such as 'an infrared stealth structure material with a multi-coating structure' (CN109046906A), and provides a method for coating Fe-containing on the surface of the material by adopting a spraying method3O4The polyaniline coating of the particles is coated with the polyurethane coating of Al again to form the infrared stealth material with a multi-coating structure, so that the infrared emissivity of the material is reduced. Although the method can reduce the infrared emissivity of the material to a certain extent, the process steps are complex, the coating can increase the weight of the whole structure, and the coating and the substrate material are in a risk of peeling.
Disclosure of Invention
The invention provides a method for reducing the infrared emissivity of a polyimide resin matrix composite material, which is designed and provided aiming at the problems in the prior art. The surface of the polyimide resin matrix composite material is modified, so that a metal silver layer can be formed on the surface of the polyimide resin matrix composite material through simple heating post-treatment, and the infrared emissivity of the polyimide resin matrix composite material is reduced. The method has the advantages of no need of excessive complicated process steps, simple process, low cost, obvious reduction of infrared emissivity and no obvious weight increase.
The purpose of the invention is realized by the following technical scheme:
the method for reducing the infrared emissivity of the polyimide resin matrix composite material comprises the following steps:
firstly, etching the surface of the polyimide resin matrix composite material by using an alkaline solution, and leaching the surface of the polyimide resin matrix composite material to a pH value within a range of 7-8 by using deionized water after etching;
step two, preparing a silver nitrate solution with the concentration of 0.4 mol/L;
step three, immersing the polyimide resin-based composite material subjected to surface etching in the step one into the silver nitrate solution in the step two for ion exchange, and leaching the surface by using deionized water after the ion exchange is finished to obtain a surface modified polyimide resin-based composite material;
and step four, heating the surface modified polyimide resin matrix composite material obtained in the step three, and then processing to obtain the low infrared emissivity polyimide resin matrix composite material.
In one implementation, the alkaline solution in the first step is sodium hydroxide solution or potassium hydroxide solution, and the concentration is 4 mol/L.
In one implementation, the alkaline etching process in the step one is completed under the constant temperature condition of 25 ℃, and the etching time is 11-24 h.
Further, the alkali liquor etching process in the step one is completed under the constant temperature condition of 25 ℃, and the etching time is 11 hours.
Further, the alkali liquor etching process in the step one is completed under the constant temperature condition of 25 ℃, and the etching time is 22 hours.
In one implementation, the ion exchange process in the third step is completed under the constant temperature condition of 25 ℃, and the ion exchange time is 5-24 h.
In one embodiment, the heat post-treatment process in the fourth step is a constant temperature condition of 135 ℃ for 1 hour.
In one embodiment, the heat post-treatment process in step four comprises: heating to 135 deg.C for 1h, maintaining the temperature at 135 deg.C for 1h, heating to 350 deg.C for 2h, and maintaining the temperature at 350 deg.C for 2 h.
The technical scheme of the invention has the characteristics and advantages that:
compared with the existing method for reducing the infrared emissivity of the composite material by spraying the infrared stealth coating material on the surface of the base material, the method has the advantages that the surface treatment process of the polyimide resin matrix composite material is simple, the etching process only needs to soak the polyimide resin matrix composite material in a strong alkaline solution at a constant temperature, and the post-treatment process can be completed only by simple heating treatment. The silver layer formed on the surface of the polyimide resin-based composite material by the method has no obvious weight increase on the whole structure, is tightly combined with the matrix, and has small stripping risk. The infrared emissivity of the material treated by the method is obviously reduced, for example, the infrared emissivity of the untreated polyimide composite material is 0.528 at the wavelength range of 3-5 mu m and 0.541 at the wavelength range of 8-14 mu m. The infrared emissivity of the polyimide composite material treated by the method is 0.315 at the wavelength range of 3-5 mu m and 0.299 at the wavelength range of 8-14 mu m. The method provided by the invention can be used for reducing the infrared emissivity of the polyimide resin matrix composite material, so that the requirement of infrared stealth performance is met.
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FIG. 1 is a view showing the surface of a polyimide resin-based composite material which has not been treated (a) in comparative example and which has been treated (b) in example 1 by the present method.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The materials are commercially available from the open literature unless otherwise specified.
Example 1:
the method for reducing the infrared emissivity of the polyimide resin matrix composite material comprises the following steps:
(1) and (2) immersing the polyimide resin matrix composite material into a sodium hydroxide solution with the concentration of 4mol/L, etching for 11 hours at the constant temperature of 25 ℃, and leaching the surface of the polyimide resin matrix composite material to the pH value of 7-8 by using deionized water after etching.
(2) Mixing silver nitrate (AgNO)3) Dissolving in deionized water to obtain silver nitrate solution with the concentration of 0.4 mol/L.
(3) And (2) immersing the polyimide resin matrix composite material with the etched surface in the step (1) into the silver nitrate solution in the step (2), carrying out ion exchange for 24 hours at the constant temperature of 25 ℃, and leaching the surface by using deionized water after the ion exchange is finished to obtain the surface modified polyimide resin matrix composite material.
(4) And (4) heating the surface modified polyimide resin matrix composite material in the step (3) and then processing to obtain the low infrared emissivity polyimide resin matrix composite material. The post-treatment process comprises the following steps: heating to 135 deg.C for 1h, maintaining the temperature at 135 deg.C for 1h, heating to 350 deg.C for 2h, and maintaining the temperature at 350 deg.C for 2 h. The infrared emissivity of the polyimide composite material treated by the method at the wavelength ranges of 3-5 μm and 8-14 μm is shown in Table 1.
Example 2:
the method for reducing the infrared emissivity of the polyimide resin matrix composite material comprises the following steps:
(1) soaking the polyimide resin matrix composite material into a sodium hydroxide solution with the concentration of 4mol/L, etching for 22 hours at the constant temperature of 25 ℃, and leaching the surface of the polyimide resin matrix composite material by using deionized water until the pH value is neutral.
(2) Mixing silver nitrate (AgNO)3) Dissolving in deionized water to obtain silver nitrate solution with the concentration of 0.4 mol/L.
(3) And (2) immersing the polyimide resin matrix composite material with the etched surface in the step (1) into the silver nitrate solution in the step (2), carrying out ion exchange for 5 hours at the constant temperature of 25 ℃, and leaching the surface by using deionized water after the ion exchange is finished to obtain the surface modified polyimide resin matrix composite material.
(4) And (4) heating the surface modified polyimide resin matrix composite material in the step (3) and then processing to obtain the low infrared emissivity polyimide resin matrix composite material. The post-treatment process comprises the following steps: heating to 135 deg.C for 1h, maintaining the temperature at 135 deg.C for 1h, heating to 350 deg.C for 2h, and maintaining the temperature at 350 deg.C for 2 h. The infrared emissivity of the polyimide composite material treated by the method at the wavelength ranges of 3-5 μm and 8-14 μm is shown in Table 1.
Comparative example:
the infrared emissivity measured directly at the wavelength ranges of 3 to 5 μm and 8 to 14 μm without any treatment using the same polyimide composite as the polyimide composite described in examples 1 and 2 is shown in Table 1.
FIG. 1 is a surface of a polyimide resin based composite material untreated in comparative example and treated in example 1 by the method described in this patent, and it can be seen that the surface of the polyimide resin based composite material subjected to surface etching and ion exchange treatment produced a distinct silver layer (FIG. 1 b). The infrared emissivity of the polyimide resin-based composite materials in the examples and comparative examples at the wavelength ranges of 3 to 5 μm and 8 to 14 μm are shown in Table 1. As can be seen from Table 1, compared with the comparative example, the surface-etched and ion-exchanged polyimide resin-based composite material has significantly reduced infrared emissivity in the two wave band ranges of 3-5 μm and 8-14 μm. For example, the infrared emissivity of the polyimide resin matrix composite material etched for 22 hours and ion exchange for 5 hours at a constant temperature of 25 ℃ is 0.240 and 0.251 at the wavelength ranges of 3-5 μm and 8-14 μm, which are respectively reduced by 54.55% and 53.60% compared with the untreated polyimide resin matrix composite material. The method provided by the invention can effectively reduce the infrared emissivity of the polyimide resin matrix composite material.
TABLE 1 Infrared emissivity of polyimide resin based composites
| Examples | 3～5μm | 8～14μm |
| Example 1 | 0.315 | 0.299 |
| Example 2 | 0.240 | 0.251 |
| Comparative example | 0.528 | 0.541 |
Claims (8)
1. A method for reducing the infrared emissivity of a polyimide resin matrix composite material is characterized by comprising the following steps: the method comprises the following steps:
firstly, etching the surface of the polyimide resin matrix composite material by using an alkaline solution, and leaching the surface of the polyimide resin matrix composite material to a pH value within a range of 7-8 by using deionized water after etching;
step two, preparing a silver nitrate solution with the concentration of 0.4 mol/L;
step three, immersing the polyimide resin-based composite material subjected to surface etching in the step one into the silver nitrate solution in the step two for ion exchange, and leaching the surface by using deionized water after the ion exchange is finished to obtain a surface modified polyimide resin-based composite material;
and step four, heating the surface modified polyimide resin matrix composite material obtained in the step three, and then processing to obtain the low infrared emissivity polyimide resin matrix composite material.
2. The method of reducing the ir-emissivity of a polyimide resin based composite material of claim 1, wherein: the alkaline solution in the first step is a sodium hydroxide solution or a potassium hydroxide solution, and the concentration is 4 mol/L.
3. The method of reducing the ir-emissivity of a polyimide resin based composite material of claim 1, wherein: the alkali liquor etching process in the step one is completed under the constant temperature condition of 25 ℃, and the etching time is 11-24 h.
4. A method for reducing the ir-emissivity of a polyimide resin based composite material according to claim 1 or 3, wherein: the alkali liquor etching process in the step one is completed under the constant temperature condition of 25 ℃, and the etching time is 11 hours.
5. A method for reducing the ir-emissivity of a polyimide resin based composite material according to claim 1 or 3, wherein: the alkali liquor etching process in the step one is completed under the constant temperature condition of 25 ℃, and the etching time is 22 h.
6. The method of reducing the ir-emissivity of a polyimide resin based composite material of claim 1, wherein: the ion exchange process in the third step is completed under the condition of constant temperature of 25 ℃, and the ion exchange time is 5-24 h.
7. The method of reducing the ir-emissivity of a polyimide resin based composite material of claim 1, wherein: the process of the heating post-treatment in the fourth step is to keep the temperature for 1 hour at the constant temperature of 135 ℃.
8. The method of reducing the ir-emissivity of a polyimide resin based composite material of claim 1, wherein: the process of the heating post-treatment in the fourth step comprises the following steps: heating to 135 deg.C for 1h, maintaining the temperature at 135 deg.C for 1h, heating to 350 deg.C for 2h, and maintaining the temperature at 350 deg.C for 2 h.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803312A (en) * | 2005-01-14 | 2006-07-19 | 北京化工大学 | Preparation method of double-surface high-reflection high conductivity polyimide/silver film |
| CN108441108A (en) * | 2018-03-22 | 2018-08-24 | 南京大学 | A kind of low infrared emissivity is compatible with the composite coating and preparation method thereof of low laser reflectivity |
| CN109046906A (en) * | 2018-07-19 | 2018-12-21 | 南昌航空大学 | A kind of multicoat structure Infrared stealthy materials |
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2020
- 2020-07-08 CN CN202010654377.4A patent/CN111944181A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1803312A (en) * | 2005-01-14 | 2006-07-19 | 北京化工大学 | Preparation method of double-surface high-reflection high conductivity polyimide/silver film |
| CN108441108A (en) * | 2018-03-22 | 2018-08-24 | 南京大学 | A kind of low infrared emissivity is compatible with the composite coating and preparation method thereof of low laser reflectivity |
| CN109046906A (en) * | 2018-07-19 | 2018-12-21 | 南昌航空大学 | A kind of multicoat structure Infrared stealthy materials |
Non-Patent Citations (2)
| Title |
|---|
| 叶盛祥主编: "《光电干扰防护系统技术》", 31 December 2005 * |
| 周遵宁编著: "《光电对抗材料基础》", 31 January 2017 * |
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