CN112530618B - Neutron irradiation resistant protective material for electronic component and preparation method thereof - Google Patents
Neutron irradiation resistant protective material for electronic component and preparation method thereof Download PDFInfo
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- CN112530618B CN112530618B CN202011346447.6A CN202011346447A CN112530618B CN 112530618 B CN112530618 B CN 112530618B CN 202011346447 A CN202011346447 A CN 202011346447A CN 112530618 B CN112530618 B CN 112530618B
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- protective material
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/12—Laminated shielding materials
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
- G21F1/00—Shielding characterised by the composition of the materials
- G21F1/12—Laminated shielding materials
- G21F1/125—Laminated shielding materials comprising metals
Abstract
A neutron irradiation resistant protective material for electronic components 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 that the existing irradiation shielding material is thick, so that the spacecraft load is too heavy, and the irradiation resistance is low due to uneven dispersion of the functional filler of the coating of the traditional blending system. The neutron irradiation resistant protective material for the electronic component is formed by alternately stacking resin bridging layers and functional metal layers, and the outermost layer is the functional metal layer. The preparation method comprises the following steps: firstly, preparing a resin coupling layer by thermal spraying and segmented curing; secondly, plating a functional metal layer on the resin bridging layer in the first step by adopting a magnetron sputtering technology and taking rare earth metal elements as targets; and thirdly, alternately repeating for 10-30 times to enable the outermost layer of the protective material to be a functional metal layer, so as to obtain the irradiation protective material. The radiation shielding rate of the protective material is up to 87.7% under the neutron 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 neutron irradiation resistant protective material for an electronic component and a preparation method thereof.
Background
The space radiation environment is one of important environmental elements faced by the on-orbit operation of the spacecraft and is also an important reason for causing the abnormity or the failure of the aerospace electronic components. The neutron radiation is uncharged, so that the neutron radiation has very strong penetrating power to substances and causes more damage to devices than other rays with the same measurement. In order to prevent the damage caused by the radiation, a special anti-neutron irradiation reinforcement treatment process is needed to ensure the on-orbit service reliability of the spacecraft, so that the research on the protective material for the neutron irradiation becomes an important research subject.
At present, the basic method of neutron radiation protection is to control the radiation dose by shielding through a physical method. Most of the existing shielding materials are made of heavy metals and other materials, and need thick thickness to achieve a certain shielding effect, so that a certain gap can be formed during installation and use, and the problems of overweight load of a spacecraft and the like also exist. In order to meet the protection requirement of electronic components with complex shapes, the thickness of materials must be reduced, so that the materials are light. Therefore, a special material with excellent radiation shielding performance, mechanical property and construction performance is required on the surface of the electronic component.
Disclosure of Invention
The invention aims to solve the technical problems that the loading of a spacecraft is too heavy due to the thicker existing radiation shielding material and the irradiation resistance of a coating is low due to the uneven dispersion of functional fillers of the coating of a traditional blending system, and provides a neutron irradiation resistant protective material for electronic components and a preparation method thereof.
The neutron irradiation resistant protective material for the electronic component is formed by alternately stacking resin bridging layers and functional metal layers, and the outermost layer is the functional metal layer.
Further, the resin bonding layer and the functional metal layer are alternately stacked for 10 to 30 cycles.
Further limited, the thickness of the resin bridging monolayer is 50-100 μm, and the thickness of the functional metal layer monolayer is 30-50 μm.
Further defined, the functional metal layer is a rare earth metal layer.
Further limit, the rare earth metal is one or a mixture of several of cerium, gadolinium and erbium according to any ratio.
The preparation method of the neutron irradiation resistant protective material for the electronic component comprises the following steps:
firstly, preparing a resin bridging layer: heating epoxy resin to a molten state, adding an accelerator and polyetherimide, uniformly mixing under a stirring state to obtain epoxy resin diluent, carrying out ultrasonic treatment on the obtained epoxy resin diluent, standing after the ultrasonic treatment, then spraying the standing epoxy resin diluent on the surface of a tube shell of an electronic component, and then carrying out segmented curing to obtain a resin coupling layer;
secondly, preparing a functional metal layer: by adopting magnetron sputtering technology, rare earth metal elements are used as target materials, argon is used as protective gas, and the vacuum degree of the back bottom is 4.5 multiplied by 10-4Pa～5.5×10-4Plating a functional metal layer on the resin bonding layer in the first step under the condition of Pa;
thirdly, alternately stacking: and alternately repeating the operation of the first step and the operation of the second step for 10-30 times, and finishing the alternate and repeated operation by the operation of the second step to enable the outermost layer of the protective material to be a functional metal layer to obtain the protective material.
Further limiting, in the step one, the epoxy resin is heated to a molten state at 70-90 ℃.
Further limiting, in the step one, the mass ratio of the epoxy resin to the accelerator is 10: (0.5 to 1).
Further limiting, in the first step, the mass ratio of the epoxy resin to the polyetherimide is 10: (1-2).
Further, in the first step, the promoter is aluminum acetylacetonate.
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 limiting, the parameters of the spraying in the first step are specifically: the diameter of the nozzle is 1 mm-3 mm, the pressure of the spray gun is 0.6 MPa-0.8 MPa, the moving speed of the spray gun is 50 cm/s-100 cm/s, and the spray distance is 10 cm-20 cm.
Further, the step one, the step of the segmented curing 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 ℃.
Further limiting, the parameters of magnetron sputtering in the step two are specifically: the sputtering power is 50W-120W, the sputtering time is 1 h-3 h, and the sputtering pressure is 0.5 Pa-1.5 Pa.
Further limiting, in the second step, the target material is one or a combination of any several of a cerium target, a gadolinium target and an erbium target.
Further limiting, the diameter of the target in the second step is 40 mm-60 mm.
Further limiting, the target distance in the step two is 100 mm-200 mm.
Further limiting, the flow rate of the argon gas in the second step is 10sccm to 30 sccm.
Compared with the prior art, the invention has the advantages that:
the invention enhances the overall mechanical property of the coating by the organic-inorganic laminated structure formed by the resin bridging layer and the functional metal layer in turn, and can effectively overcome the problem of low irradiation resistance of the coating caused by uneven dispersion of the functional filler of the traditional blended system coating.
The composite film layer structure with density gradient distribution is constructed by sequentially and alternately arranging the resin bridging layer and the functional metal layer, and the combination capability of the coating material and the matrix is favorably improved by compounding materials with different densities.
The resin bridging layer can effectively weaken rays, has good moderating effect on neutrons, simultaneously meets the supporting and protecting effects on the functional metal layer, and can enable the radiation-resistant composite material to have winding flexibility in the processing and using processes.
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 functional metal layer forms a compact tiled network structure which can be used as an electronic rapid transmission channel, can fully absorb rays, effectively improves the overall anti-irradiation performance of the composite material, and realizes the space anti-radiation reinforcement of electronic components.
The radiation shielding rate of the protective material is up to 87.7% under the neutron irradiation with the simulated dose of 100-200 kGy.
Detailed Description
The first embodiment is as follows: the neutron irradiation resistant protective material for the electronic component is formed by alternately stacking the resin bridging layers and the functional metal layers, the outermost layer is the functional metal layer, the resin bridging layers and the functional metal layers are alternately stacked for 10 cycles, the single-layer thickness of the resin bridging layers is 60 micrometers, the single-layer thickness of the functional metal layers is 40 micrometers, the functional metal layers are rare earth metal layers, and the rare earth metal is gadolinium.
The method for preparing the neutron irradiation resistant protective material for the electronic component comprises the following steps:
firstly, preparing a resin bridging layer: heating 100g of E51 type epoxy resin to a molten state at 80 ℃, adding 5.1g of aluminum acetylacetonate and 12.5g of polyetherimide, uniformly mixing under stirring to obtain epoxy resin diluent, carrying out ultrasonic treatment on the obtained epoxy resin diluent, wherein the ultrasonic power of the ultrasonic treatment is 1500W, the ultrasonic treatment is carried out for 15min, standing for 5min after ultrasonic treatment, then spraying the epoxy resin diluent after standing on the surface of an electronic component, the diameter of a nozzle is 2.7mm, the pressure of a spray gun is 0.8Mpa, the moving speed of the spray gun is 100cm/s, the spraying distance is 20cm, then carrying out segmented curing, firstly curing for 6h at 50 ℃ in a vacuum drying oven, then curing for 1h at 100 ℃, and finally curing for 1h at 130 ℃. Obtaining a resin bonding layer;
secondly, preparing a functional metal layer: adopting magnetron sputtering technology, taking gadolinium target as target material, argon as protective gas, and vacuum degree of backing at 5.0 × 10-4Plating a functional metal layer on the resin bonding layer in the first step under the condition of Pa; the magnetron sputtering parameters are as follows: the sputtering power is 50W, the sputtering time is 3h, and the sputtering pressure is 0.5 Pa; the diameter of the target is 50mm, the target distance is 150mm, and the flow rate of argon gas is 20 sccm.
Thirdly, alternately stacking: and alternately repeating the operation of the first step and the operation of the second step for 10 times, and finishing the alternate and repeated operation by the operation of the second step to enable the outermost layer of the protective material to be a functional metal layer to obtain the protective material.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the resin bridge layers and the functional metal layers are alternately stacked for 20 cycles. 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 resin bridge layers and the functional metal layers are alternately stacked for 30 cycles. 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 rare earth metal is cerium. 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 rare earth metal is erbium. 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
Radiation shielding tests were performed on the conformal coatings of embodiments one through five, with specific test parameters and results shown in table 1.
TABLE 1 irradiation screening test Table
| Neutron irradiation dose (kGy) | Irradiation time (min) | Total dose measured after irradiation (kGy) | Shielding ratio (%) | |
| Detailed description of the invention | 150 | 120 | 27.0 | 82.0 |
| Detailed description of the invention | 150 | 120 | 18.5 | 87.7 |
| Detailed description of the invention | 150 | 120 | 22.1 | 85.3 |
| Detailed description of the invention | 150 | 120 | 27.8 | 81.5 |
| Detailed description of the invention | 150 | 120 | 28.8 | 80.8 |
Claims (6)
1. The preparation method of the neutron irradiation resistant protective material for the electronic component is characterized in that the protective material is formed by alternately stacking resin bridging layers and functional metal layers, the outermost layer is the functional metal layer, the resin bridging layers and the functional metal layers are alternately stacked for 10-30 cycles, the single-layer thickness of the resin bridging layers is 50-100 mu m, the single-layer thickness of the functional metal layers is 30-50 mu m, the functional metal layers are rare earth metal layers, and the rare earth metal is one or a mixture of cerium, gadolinium and erbium;
the preparation method of the protective material comprises the following steps:
firstly, preparing a resin bridging layer: heating epoxy resin to a molten state, adding an accelerator and polyetherimide, uniformly mixing under a stirring state to obtain epoxy resin diluent, carrying out ultrasonic treatment on the obtained epoxy resin diluent, standing after the ultrasonic treatment, then spraying the standing epoxy resin diluent on the surface of a tube shell of an electronic component, and then carrying out segmented curing to obtain a resin coupling layer;
secondly, preparing a functional metal layer: by adopting magnetron sputtering technology, rare earth metal elements are used as target materials, argon is used as protective gas, and the degree of vacuum of the back bottom is 4.5 multiplied by 10-4Pa～5.5×10-4Plating a functional metal layer on the resin bonding layer in the first step under the condition of Pa;
thirdly, alternately stacking: and (5) alternately repeating the operation of the first step and the operation of the second step, and finishing the alternate and repeated operation by the operation of the second step to enable the outermost layer of the protective material to be a functional metal layer to obtain the protective material.
2. The preparation method of the neutron irradiation resistant protective material for the electronic component as claimed in claim 1, wherein in the first step, the epoxy resin is heated to a molten state at 70-90 ℃, and the mass ratio of the epoxy resin to the accelerator in the first step is 10: (0.5-1), wherein the mass ratio of the epoxy resin to the polyetherimide in the step one is 10: (1-2), wherein the accelerant in the first step is aluminum acetylacetonate.
3. The method for preparing the neutron irradiation resistant protective material for the electronic component as claimed in claim 1, wherein 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 protective material is allowed to stand for 3 min-5 min after the ultrasonic treatment.
4. The method for preparing the neutron irradiation resistant protective material for the electronic component according to claim 1, wherein the spraying parameters in the first step are as follows: the diameter of a nozzle is 1 mm-3 mm, the pressure of a spray gun is 0.6 MPa-0.8 MPa, the moving speed of the spray gun is 50 cm/s-100 cm/s, the spray distance is 10 cm-20 cm, and the segmented curing process in the step one specifically comprises the following steps: 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 ℃.
5. The method for preparing the neutron irradiation resistant protective material for the electronic component according to claim 1, wherein the parameters of the magnetron sputtering in the step two are specifically as follows: the sputtering power is 50W-120W, the sputtering time is 1 h-3 h, and the sputtering pressure is 0.5 Pa-1.5 Pa.
6. The method for preparing the neutron irradiation resistant protective material for the electronic component according to claim 1, wherein the target material in the second step is one or a combination of any more of a cerium target, a gadolinium target and an erbium target, the diameter of the target material in the second step is 40 mm-60 mm, the target distance in the second step is 100 mm-200 mm, and the flow rate of argon gas in the second step is 10 sccm-30 sccm.
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| US4644171A (en) * | 1985-04-01 | 1987-02-17 | Aar Corporation | Neutron absorbing panel |
| US5324952A (en) * | 1992-07-10 | 1994-06-28 | Ball Corporation | Radiation shielding for spacecraft components |
| US9640288B1 (en) * | 2015-11-30 | 2017-05-02 | Space Systems/Loral, Llc | Flexible radiation shield |
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