CN115304982B - Packaging shielding coating for spaceborne integrated circuit and preparation method thereof - Google Patents
Packaging shielding coating for spaceborne integrated circuit and preparation method thereof Download PDFInfo
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- CN115304982B CN115304982B CN202210962526.2A CN202210962526A CN115304982B CN 115304982 B CN115304982 B CN 115304982B CN 202210962526 A CN202210962526 A CN 202210962526A CN 115304982 B CN115304982 B CN 115304982B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
- C09D123/02—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D123/04—Homopolymers or copolymers of ethene
- C09D123/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D179/00—Coating compositions based on 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 C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
- G21F1/02—Selection of uniform shielding materials
- G21F1/023—Liquids
-
- 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
- G21F1/02—Selection of uniform shielding materials
- G21F1/10—Organic substances; Dispersions in organic carriers
- G21F1/103—Dispersions in organic carriers
Abstract
The invention discloses a packaging shielding coating for a satellite-borne integrated circuit and a preparation method thereof, belongs to the technical field of functional material preparation, and particularly relates to the technical field of special functional coatings. The invention solves the defects of high cost, high density, poor mechanical property and the like of the traditional radiation-resistant shielding material. The invention combines the lead halogen perovskite powder with the resin material, combines the advantages of each component material, constructs a composite coating with excellent properties, and simultaneously realizes the shielding of various high-energy rays and inhibits the generation of secondary particles by utilizing the mode of the cooperation of the lead halogen perovskite powder multi-component material. And a large number of interfaces of lead halogen perovskite and resin exist in the composite coating, so that a structure with alternately arranged high-low Z materials is constructed, and the bremsstrahlung generated by the action of high-energy electrons and the high-Z materials is further inhibited.
Description
Technical Field
The invention relates to a packaging shielding coating for a satellite-borne integrated circuit and a preparation method thereof, belongs to the technical field of functional material preparation, and particularly relates to the technical field of special functional coatings.
Background
With the comprehensive development of Mars detection tasks, deep space detection enters a new era, and higher requirements are put on the service life of a satellite-borne integrated circuit. The space-borne integrated circuit is in a severe space radiation environment at any time, wherein high-energy rays such as high-energy electrons and gamma rays can generate total dose effect, single event effect, displacement effect and other radiation effects in the space-borne integrated circuit, so that the working stability of the space-borne integrated circuit is seriously influenced, even the space-borne integrated circuit is damaged, and the service life of the space-borne integrated circuit is shortened. Therefore, it is important to develop and design a shielding coating for a package of a satellite-borne integrated circuit with excellent radiation shielding properties.
The existing shielding material is mainly selected by considering the materials with high atomic number and high density, lead metal is used as a traditional radiation shielding material, and the traditional radiation shielding material is widely applied to the fields of nuclear industry, nuclear medicine and the like, but the traditional radiation shielding material is toxic in lead, serious in environmental pollution, poor in shielding performance on an X-ray due to a weak absorption area, high in quality and poor in mechanical performance, and is not suitable for being used as a packaging shielding coating of a satellite-borne integrated circuit. Therefore, it is necessary to provide a composite coating with light weight, excellent radiation shielding performance and good mechanical performance for packaging shielding coatings of satellite-borne integrated circuits.
Disclosure of Invention
The invention provides a composite coating with light weight, excellent radiation shielding performance and good mechanical performance for packaging a space-borne integrated circuit and a preparation method thereof, which aims to solve the defects of high cost, high density, poor mechanical performance and the like of the traditional radiation-resistant shielding material.
The technical scheme of the invention is as follows:
one of the objects of the present invention is to provide a method for preparing a radiation shielding coating, comprising the steps of:
s1, preparing lead halide perovskite powder;
lead salt, halogen acid and methylamine are used as raw materials, and lead halogen perovskite powder is prepared by a solvothermal method;
s2, preparing a composite coating;
mixing lead halogen perovskite powder with resin, grinding to obtain slurry, coating the slurry on the surface of an object to be protected, and curing to form the radiation shielding coating.
Further defined, the lead salt in S1 is lead acetate and/or lead iodide.
Further defined, the hydrohalic acid in S1 is hydrochloric acid, hydrobromic acid or hydroiodic acid.
Further defined, S1 operates specifically as: adding lead salt into halogen acid solution, stirring until the lead salt is completely dissolved, adding isopropanol solvent, stirring uniformly, adding methylamine solution, transferring the mixed solution into a reaction kettle, heating for reaction, and sequentially carrying out centrifugation, washing and drying after the reaction is finished to obtain lead halogen perovskite powder.
Further limited, the heating reaction temperature is 60-180 ℃ and the time is 0.5-4 h.
Further limited, the mass ratio of the lead halogen perovskite powder to the resin in the S2 is (1-3) to (7-9).
Further defined, the resin in S2 is an epoxy, polyethylene, polyurethane or cyanate.
Further selecting, grinding in the step S2, wherein a three-roller grinder is adopted, and the grinding time is 5-20 min.
Further defined, the slurry application means includes, but is not limited to, knife coating, brush coating, spray coating, or spin coating.
Further defined, the thickness of the slurry applied to the surface of the object to be protected is 100 μm to 500 μm.
Further limited, the curing treatment temperature is 60-150 ℃ and the curing treatment time is 2-8 h.
It is an object of the present invention to provide a radiation shielding coating prepared by the above method for use in encapsulation shielding coatings for on-board integrated circuits.
The invention combines the lead halogen perovskite powder with the resin material, combines the advantages of each component material, constructs a composite coating with excellent properties, and simultaneously realizes the shielding of various high-energy rays and inhibits the generation of secondary particles by utilizing the mode of the cooperation of the lead halogen perovskite powder multi-component material. Compared with the prior art, the application has the following beneficial effects:
(1) The invention embeds the lead halogen perovskite powder into the resin material, effectively controls the density of the composite coating, prepares the light composite coating, and effectively solves the defects of high lead metal density, high toxicity and the like of the traditional material.
(2) The lead halogen perovskite powder prepared by the method constructs a blocking channel in the resin matrix, enhances the collision probability between gamma rays and materials, and effectively attenuates the intensity of incident gamma rays. In addition, methylamine ions in lead halogen perovskite lattices can block further transmission of secondary electrons, shorten penetration depth of the secondary electrons, have good protective capability on high-energy electrons, and meanwhile, the resin material can serve as a moderator to slow down neutrons.
(3) And a large number of interfaces of lead halogen perovskite and resin exist in the composite coating prepared by the invention, so that a structure with alternately arranged high-low Z materials is constructed, and the bremsstrahlung generated by the action of high-energy electrons and the high-Z materials is inhibited to a certain extent.
(4) The lead halogen perovskite powder prepared by the invention can also play a role in enhancing mechanical properties on a resin matrix.
(5) The preparation process of the composite coating provided by the invention is simple and is suitable for mass production.
Drawings
FIG. 1 shows the powder of lead-halogenite-perovskite powder (MAPbBr) prepared in example 1 3 ) SEM photographs of (2);
FIG. 2 shows a composite coating (MAPbBr) prepared in example 1 3 +epoxy);
FIG. 3 shows the powder of lead-halogenite-perovskite powder (MAPbBr) prepared in example 1 3 ) And composite coating (MAPbBr) 3 +epoxy resin);
FIG. 4 is a simulation of the penetration depth of electrons in an epoxy;
FIG. 5 shows an electron in a composite coating (MAPbBr) 3 +epoxy) penetration depth simulation;
FIG. 6 shows an electron in composite coating (PbBr) 2 +epoxy) penetration depth simulation;
FIG. 7 shows lead prepared in example 2Calcium halide titanium ore powder (MAPbI) 3 ) SEM photographs of (2);
FIG. 8 shows a composite coating (MAPbI) prepared in example 2 3 +epoxy).
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified. The materials, reagents, methods and apparatus used, without any particular description, are those conventional in the art and are commercially available to those skilled in the art.
Example 1:
this example prepares a composite coating (MAPbBr) 3 +epoxy resin) is carried out according to the following steps:
step 1, preparing lead halogen perovskite powder (MAPbBr) 3 )：
Firstly, accurately weighing 120mg of lead white acetate trihydrate powder in a clean beaker, adding 2mL of hydrobromic acid solution with the concentration of 50wt% into the beaker, stirring until the powder is completely dissolved in the hydrobromic acid solution, adding 60mL of isopropanol solvent into the beaker, uniformly stirring, adding 600 mu L of methylamine solution with the concentration of 30wt% into the beaker by using a pipette, and continuously stirring for 30min. Secondly, pouring the prepared mixed precursor into a lining of a polytetrafluoroethylene reaction kettle with the volume of 100mL, loading the lining into a reaction kettle, placing the lining into an oven, preserving heat for 4 hours at the temperature of 140 ℃, taking out the reaction kettle, cooling to room temperature, centrifuging a reaction product, continuously washing the reaction product with an isopropanol solution for 3 times, and drying to obtain lead halogen perovskite powder (MAPbBr) 3 )。
For the obtained lead halogen perovskite powder (MAPbBr) 3 ) The microscopic morphology characterization is carried out, the result is shown in figure 1, and the prepared MAPbBr is shown in the figure 3 The powder is in a cube shape and has a complete crystal structure.
For obtaining lead halogen perovskite powder (MAP)bBr 3 ) XRD testing was performed and the results are shown in FIG. 3 as MAPbBr 3 As shown in the graph, the diffraction peaks of the prepared powder XRD at 14.9 degrees, 21.2 degrees, 30.2 degrees, 33.8 degrees, 37.2 degrees, 43.2 degrees, 45.9 degrees, 48.6 degrees, 53.6 degrees, 55.9 degrees and 58.2 degrees respectively correspond to (100), (110), (200), (210), (211), (220), (300), (310), (222), (320) and (321) crystal faces, which shows that MAPbBr is successfully prepared 3 And (3) powder. .
Step 2, preparing a composite coating (MAPbBr 3 + epoxy resin):
the lead halogen perovskite powder (MAPbBr) obtained above was then mixed with 3 ) Mixing with epoxy resin (mixing agent K-9761A and agent B according to mass ratio of 2:1), wherein the lead halogen perovskite powder (MAPbBr) 3 ) The mass ratio of the epoxy resin to the epoxy resin is 1:9. fully grinding the mixture of the two by using a three-roller grinder for 10min, coating the obtained slurry on the surface of the satellite-borne integrated circuit by adopting a blade coating mode after grinding to form a coating with the thickness of 500 mu m, placing the coating in a vacuum drying oven, and curing for 6h at the temperature of 60 ℃ to obtain a composite coating (MAPbBr) 3 +epoxy resin).
For the composite coating obtained (MAPbBr 3 +epoxy resin) was subjected to microscopic morphological characterization, and the results are shown in FIG. 2, from which MAPbBr can be seen 3 The powder is uniformly dispersed in the epoxy resin.
For the composite coating obtained (MAPbBr 3 +epoxy resin) was subjected to XRD testing, and the results were shown as MAPbBr in FIG. 3 3 As can be seen from the graph, the XRD diffraction peak of the composite coating corresponds to MAPbBr 3 Shows successful MAPbBr conversion 3 Into the epoxy resin.
For the composite coating obtained (MAPbBr 3 +epoxy resin), the composite coating was irradiated with a 241-Am source (59.5 keV) for 10s, and the test results are shown in table 1 below:
TABLE 1
As can be seen from Table 1, the density of the resulting composite coating was 1.287g/cm 3 The linear attenuation coefficient is 0.698cm -1 The composite coating with the thickness of only 0.992cm can attenuate the initial gamma rays by 50 percent, and has excellent radiation shielding performance.
For the composite coating obtained (MAPbBr 3 +epoxy resin), the results of which are shown in FIG. 5, show that the penetration depth of 59.5keV in the composite coating layer is 50 μm, and that MAPbBr is compared with the penetration depth of the electrons in the epoxy resin of FIG. 4 3 The powder is added to effectively block the penetration behavior of electrons in the composite coating.
For the composite coating obtained (MAPbBr 3 +epoxy resin) and epoxy resins were subjected to mechanical property tests, the test samples were 3 in total, and the mechanical property test results are shown in tables 2 and 3 below:
table 2:
| elastic modulus/GPa | 1 | 2 | 3 | Average value of |
| EP | 2.3 | 1.4 | 2.6 | 2.1 |
| Composite coating | 3.7 | 3.8 | 3.7 | 3.7 |
As can be seen from Table 2, MAPbBr 3 The addition of the powder promotes the elastic modulus of the composite coating.
Table 3:
as can be seen from Table 3, MAPbBr 3 The addition of the powder promotes the hardness of the composite coating.
Comparative example 1:
the differences between this comparative example and the examples are: in step 1, no methylamine solution was added, and the rest of the procedure and the parameter settings were the same as in example 1.
The obtained coating was subjected to electron penetration depth simulation, and the results are shown in fig. 6:
the composite coating formed by not adding methylamine solution is PbBr 2 +epoxy, 59.5keV penetration depth in the composite coating was 52 μm, and electron penetration in the composite coating (MAPbBr) was similar to that of FIG. 5 3 + epoxy resin), the presence of methylamine ions can block further transport of electrons.
Example 2:
this example prepares a composite coating (MAPbI 3 +epoxy resin) is carried out according to the following steps:
step 1, preparing lead halogen perovskite powder (MAPbI) 3 )：
Firstly, accurately weighing 120mg of lead acetate trihydrate white powder in a clean beaker, adding 2mL of hydriodic acid solution with the concentration of 50wt%,stirring until the powder was completely dissolved in the hydroiodic acid solution, adding 60mL of isopropanol solvent to the beaker, stirring uniformly, adding 600 μl of 30wt% methylamine solution thereto with a pipette, and stirring for 30min. Secondly, pouring the prepared mixed precursor into a 100mL polytetrafluoroethylene reaction kettle liner, loading the mixed precursor into a reaction kettle, placing the reaction kettle into an oven, preserving heat for 4 hours at 140 ℃, taking out the reaction kettle, cooling to room temperature, centrifuging a reaction product, continuously washing the reaction product with an isopropanol solution for 3 times, and drying to obtain lead halogen perovskite powder (MAPbI) 3 )。
For the obtained lead halogen perovskite powder (MAPbI) 3 ) The microscopic morphology characterization is carried out, the result is shown in figure 7, and the prepared MAPbI can be seen from the figure 3 The powder is in a cuboid shape and has a complete crystal structure.
Step 2, preparation of composite coating (MAPbI 3 + epoxy resin):
the lead halogen perovskite powder (MAPbI) obtained above was then mixed with 3 ) Mixing with epoxy resin (mixing agent K-9761A and agent B according to mass ratio of 2:1), wherein the lead halogen perovskite powder (MAPbI) 3 ) The mass ratio of the epoxy resin to the epoxy resin is 2:8. fully grinding the mixture of the two by using a three-roller grinder for 10min, coating the obtained slurry on the surface of the satellite-borne integrated circuit by adopting a blade coating mode after grinding to form a coating with the thickness of 500 mu m, placing the coating in a vacuum drying oven, and curing for 6h at the temperature of 60 ℃ to obtain a composite coating (MAPbI) 3 +epoxy resin).
For the composite coating (MAPbI) 3 +epoxy resin) was subjected to microscopic morphological characterization, and the results are shown in FIG. 8, from which MAPbI can be seen 3 The powder is uniformly dispersed in the epoxy resin.
For the composite coating (MAPbI) 3 +epoxy resin), the composite coating was irradiated with a 241-Am source (59.5 keV) for 10s, and the test results are shown in table 3 below:
table 3:
as is clear from Table 3, the density of the resulting composite coating was 1.390g/cm 3 The linear attenuation coefficient is 1.640cm -1 The composite coating with the thickness of only 0.423cm can attenuate the initial gamma rays by 50 percent, and has excellent radiation shielding performance.
While the invention has been described in terms of preferred embodiments, it is not intended to be limited thereto, but rather to enable any person skilled in the art to make various changes and modifications without departing from the spirit and scope of the present invention, which is therefore to be limited only by the appended claims.
Claims (7)
1. A method for preparing a radiation shielding coating, characterized by the steps of:
s1, preparing lead halide perovskite powder;
lead salt, halogen acid and methylamine are used as raw materials, and lead halogen perovskite powder is prepared by a solvothermal method;
s1 specifically comprises the following steps: adding lead salt into the halogen acid solution, stirring until the lead salt is completely dissolved, adding an isopropanol solvent, stirring uniformly, adding a methylamine solution, transferring the mixed solution into a reaction kettle, heating for reaction, and sequentially carrying out centrifugation, washing and drying after the reaction is finished to obtain lead halogen perovskite powder;
the heating reaction temperature is 60-180 ℃ and the time is 0.5-4 h;
s2, preparing a composite coating;
mixing lead halogen perovskite powder with resin, grinding to obtain slurry, coating the slurry on the surface of an object to be protected, and curing to form a radiation shielding coating;
the mass ratio of the lead halogen perovskite powder to the resin is (1-3) (7-9), and the resin is epoxy resin, polyethylene, polyurethane or cyanate.
2. A method of producing a radiation shielding coating according to claim 1, characterized in that the lead salt is lead acetate and/or lead iodide.
3. A method of preparing a radiation shielding coating according to claim 1, wherein the hydrohalic acid is hydrochloric acid, hydrobromic acid or hydroiodic acid.
4. The method for preparing the radiation shielding coating according to claim 1, wherein a three-roller grinder is adopted for grinding, and the grinding time is 5-20 min.
5. The method for preparing the radiation shielding coating according to claim 1, wherein the curing treatment temperature is 60-150 ℃ and the curing treatment time is 2-8 hours.
6. A radiation shielding coating prepared by the method of claim 1.
7. A radiation shielding coating as set forth in claim 6 applied to a packaging shielding coating for a space-borne integrated circuit.
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| WO2017053514A1 (en) * | 2015-09-22 | 2017-03-30 | Florida State University Research Foundation, Inc. | Organometal halide perovskite nanoplatelets, devices, and methods |
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| CN110330434A (en) * | 2019-08-02 | 2019-10-15 | 中国建材国际工程集团有限公司 | A kind of organic inorganic hybridization perovskite material and preparation method thereof |
| CN111925292A (en) * | 2020-10-13 | 2020-11-13 | 江西省科学院能源研究所 | Preparation method of perovskite microcrystal |
| CN113524658B (en) * | 2021-06-22 | 2022-12-09 | 西安交通大学 | Additive manufacturing method of light shielding body with multi-ray shielding and self-generating functions |
| CN113881312B (en) * | 2021-09-30 | 2022-06-17 | 哈尔滨工业大学 | Rare earth-high Z-graphene-composite coating for aerospace-grade chip total dose effect protection and preparation method thereof |
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| CN106867305A (en) * | 2017-02-27 | 2017-06-20 | 华中科技大学 | A kind of modified CeO in surface2Nano material and product |
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| KR20220096273A (en) * | 2020-12-30 | 2022-07-07 | 재단법인대구경북과학기술원 | Manufacturing method of perovskite nano particles-polymer composite and perovskite nano particles-polymer composite using the same |
| CN113637126A (en) * | 2021-08-03 | 2021-11-12 | 西北工业大学 | Star-polymer-doped perovskite solar cell and preparation method thereof |
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