CN112509720A - Cyanate ester radical anti-irradiation reinforced conformal coating and preparation method thereof - Google Patents
Cyanate ester radical anti-irradiation reinforced conformal coating and preparation method thereof Download PDFInfo
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- G21F1/02—Selection of uniform shielding materials
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Abstract
An cyanate ester radical irradiation-resistant reinforced conformal coating and a preparation method thereof. The invention belongs to the field of radiation shielding materials and preparation thereof. The invention aims to solve the technical problems of low protective performance and poor film bonding force of the existing radiation shielding material. The cyanate ester irradiation-resistant reinforced conformal coating is composed of a rare earth resin film layer and a metal oxide film, wherein an atomic layer of the metal oxide film is deposited on the outer surface of the rare earth resin film layer, and the rare earth resin film layer is formed by mixing, melting and coating rare earth micro powder, cyanate ester resin, an accelerator, a coupling agent and polyetherimide. The preparation method comprises the following steps: firstly, mixing and melting cyanate ester resin, an accelerator, a coupling agent, polyetherimide and rare earth micro powder, coating the mixture on the surface of a tube shell of an electronic component, and curing the mixture in sections to obtain a rare earth resin film layer; and secondly, periodically depositing and growing metal oxide on the surface of the rare earth resin film layer to obtain the conformal coating. The conformal coating has the radiation shielding rate of 88.5 percent under the electron irradiation with the simulated dose of 100-200 kGy.
Description
Technical Field
The invention belongs to the field of radiation shielding materials and preparation thereof, and particularly relates to a cyanate ester radical anti-radiation reinforced conformal coating and a preparation method thereof.
Background
The environment conditions of the spacecraft in the outer space are very harsh, and the integrated circuit can be subjected to the radiation action of a plurality of high-energy particles due to the existence of the high-energy particles in the outer space environment of the spacecraft, so that the performance of the integrated circuit is degraded. The overall dose effect, which occurs with increasing radiation dose, will further affect the performance of the integrated circuit, causing the spacecraft to malfunction or shorten its useful life. In order to reduce the harm caused by space radiation, a special anti-radiation reinforcement treatment process is required to ensure the reliability of the in-orbit service of the spacecraft.
Conformal coatings are used as a special polymeric film-forming material to protect circuit boards, components and other electronic components from adverse environmental conditions caused by corrosion and contamination. The advantages of low cost, short curing time and no release of contaminants during application are of great interest to researchers.
Disclosure of Invention
The invention aims to solve the technical problems of low protective performance and poor film bonding force of the existing radiation shielding material, and provides a cyanate ester-based anti-radiation reinforced conformal coating and a preparation method thereof.
The cyanate ester irradiation-resistant reinforced conformal coating is composed of a rare earth resin film layer and a metal oxide film layer, wherein an atomic layer is deposited on the outer surface of the rare earth resin film layer, and the rare earth resin film layer is formed by mixing, melting and coating rare earth micro powder, cyanate ester resin, an accelerator, a coupling agent and polyetherimide.
Further, the metal oxide of the metal oxide film layer is hafnium oxide, silicon oxide or aluminum oxide.
Further limited, the rare earth resin film layer is 80-200 μm, and the thickness of the metal oxide film layer is 30-60 nm.
Further limiting, the rare earth micro powder is one or a mixture of several of cerium, samarium, gadolinium and erbium according to any ratio.
Further limiting, the particle size of the rare earth micro powder is 300-500 meshes.
Further defined, the promoter is aluminum acetylacetonate.
Further defined, the coupling agent is a silane coupling agent.
Further limiting, the mass ratio of the cyanate ester resin to the rare earth micro powder is 10: (2-3).
Further limited, the mass ratio of the cyanate ester resin to the accelerator is 10: (0.5 to 1).
Further defined, the mass ratio of the cyanate ester resin to the coupling agent is 10: (0.5-0.8).
Further defined, the mass ratio of the cyanate ester resin to the polyetherimide is 10: (1-2).
The preparation method of the cyanate ester group irradiation-resistant reinforced conformal coating is carried out according to the following steps:
firstly, preparing a rare earth resin film layer: heating cyanate ester resin to a molten state, adding an accelerant, a coupling agent, polyetherimide and rare earth micro powder, uniformly mixing under a stirring state to obtain a coating diluent, carrying out ultrasonic treatment on the obtained coating diluent, standing after the ultrasonic treatment, coating the standing coating diluent on the surface of a tube shell of an integrated circuit, and then carrying out segmented curing to obtain a rare earth resin film layer;
secondly, preparing a composite conformal coating: placing the rare earth resin film layer obtained in the step one into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to a vacuum degree of 4 multiplied by 10-3Torr～6×10-3Torr, and introducing a protective atmosphere to the pressure of the cavityThe force is 0.1 Torr-0.2 Torr, then atomic layer periodic deposition is carried out under the condition that the temperature is 150-250 ℃, and a metal oxide film layer is periodically deposited and grown on the surface of the rare earth resin film layer, so as to obtain the conformal coating.
Further, in the first step, the cyanate ester resin is heated to a molten state at 70-90 ℃.
Further limiting, the ultrasonic power of the ultrasonic treatment in the step one is 1000W-2000W, the ultrasonic treatment time is 10 min-20 min, and the ultrasonic treatment is followed by standing for 3 min-5 min.
Further defined, the coating in step one is spin coating, blade coating or spray coating.
Further limiting, the protective atmosphere in the second step is nitrogen with the purity of 99.99%.
Further limiting, in the second step, the periodic deposition grows for 50-300 cycle periods.
Further, the metal source for the atomic layer periodic deposition growth in the second step is a hafnium source, an aluminum source or a silicon source.
Further defined, the hafnium source is tetrakis (dimethylamino) hafnium (IV), the aluminum source is trimethylaluminum, and the silicon source is tris (tert-pentaoxo) silanol.
Further limiting, in the second step, the oxygen source for the atomic layer periodic deposition growth is deionized water or ozone.
Further limiting, the temperature of the oxygen source for the atomic layer periodic deposition growth in the second step is room temperature.
Further limit is as follows: and in the second step, the thickness of the metal oxide film layer is 30 nm-60 nm.
Further limit is as follows: in the second step, the metal oxide film layer structure is distributed in a discrete island shape.
Further, the specific process of each growth and deposition cycle of the atomic layer cycle deposition in the step two is as follows: injecting an oxygen source into the deposition cavity in a pulse mode, wherein the pulse time is 0.02 s-0.04 s, then purging with nitrogen for 30 s-60 s, then injecting a metal source into the deposition cavity in a pulse mode, wherein the pulse time is 0.1 s-0.3 s, and then purging with nitrogen for 30 s-60 s.
Compared with the prior art, the invention has the advantages that:
according to the invention, the polyetherimide with low volatility is adopted to modify the main resin to form a semi-interpenetrating network structure, so that the toughness and the shear strength of the film layer can be effectively improved, and the low condensable volatility and the good bonding performance are realized. The nano oxide film is further deposited on the surface of the composite conformal coating by utilizing the atomic layer deposition technology to construct the double-layer protective composite conformal coating, so that the integral anti-irradiation performance of the coating can be effectively improved, the space anti-irradiation reinforcement of electronic components is realized, and the composite conformal coating has wide application prospect in the field of protection of exposed parts of the spacecraft.
The conformal coating constructed by the invention is formed by a two-layer structure, the atomic layer deposition technology is utilized to deposit the nano metal oxide film on the surface of the inner high rare earth content resin layer, the advantages of low deposition temperature and uniform and controllable thickness are achieved, and the interface bonding strength between the coating film layer and the substrate can be effectively improved by utilizing the good three-dimensional shape retention and wrapping performance of the nano metal oxide film.
The invention increases the oxygen vacancy in the crystal lattice by adjusting and optimizing the deposition process of the metal oxide film layer, is beneficial to the rapid transfer of electrons and can fully absorb rays. The inner layer and the outer layer are compounded by materials with different densities, so that the binding capacity of the coating material and the substrate is improved, the supporting and protecting effects on the metal oxide film layer are met, low-energy protons and low-energy neutrons can be absorbed, and the efficient absorption effect on X rays and gamma rays is also realized. The space radiation-resistant reinforcement of electronic components is realized, and technical support is provided for material selection and design of the spacecraft with long service life and high reliability.
The conformal coating has the radiation shielding rate of 88.5 percent under the electron irradiation with the simulated dose of 100-200 kGy.
Detailed Description
The first embodiment is as follows: the cyanate ester irradiation-resistant reinforced conformal coating of the embodiment comprises a rare earth resin film layer and a metal oxide film layer, wherein an atomic layer of the metal oxide film layer is deposited on the outer surface of the rare earth resin film layer, the rare earth resin film layer is formed by mixing, melting and coating rare earth micro powder, cyanate ester resin, an accelerant, a coupling agent and polyetherimide, the metal oxide of the metal oxide film layer is hafnium oxide, the thickness of the rare earth resin film layer is 120 μm, the thickness of the hafnium oxide film layer is 45nm, the rare earth micro powder is gadolinium, the particle size of the rare earth micro powder is 500 meshes, the accelerant is aluminum acetylacetonate, the coupling agent is gamma-aminopropyltriethoxysilane (namely KH-550), and the mass ratio of the cyanate ester resin to the rare earth micro powder is 5: 1, the mass ratio of the cyanate ester resin to the aluminum acetylacetonate is 15: 1, the mass ratio of the cyanate ester resin to the gamma-aminopropyltriethoxysilane is 20: 1, the mass ratio of the cyanate ester resin to the polyetherimide is 10: 1.
the method for preparing the cyanate ester group irradiation-resistant reinforced conformal coating comprises the following steps:
firstly, preparing a rare earth resin film layer: heating 100g of cyanate ester resin to a molten state at 80 ℃, adding 6.7g of aluminum acetylacetonate, 5g of KH-550, 10g of polyetherimide and 20g of gadolinium powder, uniformly mixing under a stirring state to obtain a coating diluent, carrying out ultrasonic treatment on the obtained coating diluent, wherein the ultrasonic power of the ultrasonic treatment is 1500W, the ultrasonic treatment lasts for 15min, standing for 5min after ultrasonic treatment, spin-coating the standing coating diluent on the surface of a tube shell of an electronic component, carrying out segmented curing, curing for 6h at 50 ℃ in a vacuum drying oven, curing for 1h at 100 ℃, and finally curing for 1h at 130 ℃ to obtain a rare earth resin film layer;
secondly, preparing a composite conformal coating: placing the rare earth resin film layer obtained in the step one into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to a vacuum degree of 5 multiplied by 10-3Torr, introducing nitrogen with the purity of 99.99 percent until the pressure of a cavity is 0.15Torr, then carrying out atomic layer periodic deposition under the condition that the temperature is 200 ℃, repeating 200 growth and deposition periods, and periodically depositing and growing a hafnium oxide film layer on the surface of the rare earth resin film layer to obtain a conformal coating; the specific process of each growth and deposition cycle is as follows: injecting ozone into the deposition cavity in a pulse mode, wherein the temperature of an oxygen source is room temperature, and the pulse time is 0.015s, then purging with 99.99% pure nitrogen for 60s, then injecting the metal source tetrakis (dimethylamino) hafnium into the deposition chamber in a pulse mode for 0.15s, and then purging with 99.99% pure nitrogen for 60 s.
In the second step of this embodiment, the metal oxide film layer structure is distributed in discrete islands.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the thickness of the rare earth resin film layer is 80 mu m, and the thickness of the metal oxide film layer is 30 nm. Other steps and parameters are the same as those in the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the thickness of the rare earth resin film layer is 150 mu m, and the thickness of the metal oxide film layer is 60 nm. Other steps and parameters are the same as those in the first embodiment.
The fourth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the metal source is tris (tert-pentaoxo) silanol. Other steps and parameters are the same as those in the first embodiment.
The fifth concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: the metal source is trimethylaluminum. Other steps and parameters are the same as those in the first embodiment.
The following tests were used to demonstrate the beneficial effects of the present invention
TABLE 1 irradiation screening test Table
| Electron dose (kGy) | Irradiation of radiationTime (min) | Total dose measured after irradiation (kGy) | Shielding ratio (%) | |
| Detailed description of the invention | 150 | 60 | 17.3 | 88.5 |
| Detailed description of the invention | 150 | 60 | 25.5 | 83.0 |
| Detailed description of the invention | 150 | 60 | 21.5 | 85.7 |
| Detailed description of the invention | 150 | 60 | 29.5 | 80.5 |
| Detailed description of the invention | 150 | 60 | 27.3 | 81.8 |
Claims (10)
1. The cyanate ester irradiation-resistant reinforced conformal coating is characterized by comprising a rare earth resin film layer and a metal oxide film layer, wherein an atomic layer of the metal oxide film layer is deposited on the outer surface of the rare earth resin film layer, and the rare earth resin film layer is formed by mixing, melting and coating rare earth micro powder, cyanate ester resin, an accelerator, a coupling agent and polyetherimide.
2. The cyanate ester-based irradiation-resistant reinforced conformal coating of claim 1, wherein the thickness of the rare earth resin film layer is 80 μm to 200 μm, the metal oxide of the metal oxide film layer is hafnium oxide, silicon oxide or aluminum oxide, and the thickness of the metal oxide film layer is 30nm to 60 nm.
3. The cyanate ester radical irradiation-resistant reinforced conformal coating of claim 1, wherein the rare earth micro powder is one or a mixture of cerium, samarium, gadolinium and erbium, the particle size of the rare earth micro powder is 300-500 mesh, and the mass ratio of the cyanate ester resin to the rare earth micro powder is 10: (2-3).
4. The cyanate ester irradiation-resistant reinforced conformal coating of claim 1, wherein the accelerator is aluminum acetylacetonate, the coupling agent is a silane coupling agent, and the mass ratio of the cyanate ester resin to the accelerator is 10: (0.5-1), wherein the mass ratio of the cyanate ester resin to the coupling agent is 10: (0.5-0.8), wherein the mass ratio of the cyanate ester resin to the polyetherimide is 10: (1-2).
5. The preparation method of the cyanate ester based irradiation-resistant reinforced conformal coating according to any one of claims 1to 4, which is characterized by comprising the following steps:
firstly, preparing a rare earth resin film layer: heating cyanate ester resin to a molten state, adding an accelerant, a coupling agent, polyetherimide and rare earth micro powder, uniformly mixing under a stirring state to obtain a coating diluent, carrying out ultrasonic treatment on the obtained coating diluent, standing after the ultrasonic treatment, coating the standing coating diluent on the surface of a tube shell of an integrated circuit, and then carrying out segmented curing to obtain a rare earth resin film layer;
secondly, preparing a composite conformal coating: placing the rare earth resin film layer obtained in the step one into a deposition cavity of an atomic layer deposition instrument, and pumping the deposition cavity to a vacuum degree of 4 multiplied by 10-3Torr～6×10-3And (3) Torr, introducing a protective atmosphere until the pressure of the cavity is 0.1-0.2 Torr, then carrying out atomic layer periodic deposition at the temperature of 150-250 ℃, and periodically depositing and growing a metal oxide film layer on the surface of the rare earth resin film layer to obtain the conformal coating.
6. The method for preparing the cyanate ester based irradiation-resistant reinforced conformal coating according to claim 5, wherein in the first step, the cyanate ester resin is heated to a molten state at 70-90 ℃, the ultrasonic power of the ultrasonic treatment in the first step is 1000W-2000W, the ultrasonic treatment time is 10 min-20 min, the cyanate ester resin is allowed to stand for 3 min-5 min after the ultrasonic treatment, and the step one, the step curing process specifically comprises: curing for 5-6 h at 40-60 ℃ in a vacuum drying oven, curing for 1-3 h at 90-110 ℃, and curing for 1-3 h at 120-140 ℃.
7. The method for preparing the cyanate ester based irradiation-resistant reinforced conformal coating according to claim 5, wherein the protective atmosphere in the second step is nitrogen with a purity of 99.99%, and the periodic deposition growth in the second step is 50-300 cycles.
8. The method of claim 5, wherein in step two, the metal source for the atomic layer periodic deposition growth is a hafnium source, an aluminum source or a silicon source, the hafnium source is tetrakis (dimethylamino) hafnium (IV), the aluminum source is trimethylaluminum, the silicon source is tris (tert-pentaoxo) silanol, the oxygen source for the atomic layer periodic deposition growth in step two is deionized water or ozone, and the oxygen source temperature for the atomic layer periodic deposition growth in step two is room temperature.
9. The method for preparing the cyanate ester based irradiation-resistant reinforced conformal coating of claim 5, wherein the thickness of the metal oxide film layer in the second step is 30nm to 60 nm.
10. The method for preparing the cyanate ester based irradiation-resistant reinforced conformal coating according to claim 5, wherein the specific process of each growth and deposition cycle of the atomic layer cycle deposition in the second step is as follows: injecting an oxygen source into the deposition cavity in a pulse mode, wherein the pulse time is 0.02 s-0.04 s, then purging with nitrogen for 30 s-60 s, then injecting a metal source into the deposition cavity in a pulse mode, wherein the pulse time is 0.1 s-0.3 s, and then purging with nitrogen for 30 s-60 s.
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| CN112675822A (en) * | 2020-11-26 | 2021-04-20 | 哈尔滨工业大学 | Preparation method of high-absorption high-emissivity ultra-black molecular adsorption coating |
| CN113878115A (en) * | 2021-09-30 | 2022-01-04 | 哈尔滨工业大学 | Total dose irradiation resistant power management chip and manufacturing method thereof |
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