CN109575606A - A kind of neutron shielding material and preparation method thereof - Google Patents
A kind of neutron shielding material and preparation method thereof Download PDFInfo
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- CN109575606A CN109575606A CN201811338119.4A CN201811338119A CN109575606A CN 109575606 A CN109575606 A CN 109575606A CN 201811338119 A CN201811338119 A CN 201811338119A CN 109575606 A CN109575606 A CN 109575606A
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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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Abstract
The invention discloses a kind of neutron shielding materials and preparation method thereof, by weight percentage, including matrix 20-40%, curing agent 20-40%, neutron-absorbing material 10-40%, fire retardant 1-5%, densifier 1-5%；By 3- aminopropyl triethoxysilane coupling agent, to neutron-absorbing material, its progress surface is modified, solve the problems, such as the interface compatibility of neutron-absorbing material and matrix, and using the phenyl vinyl polysiloxane of high-content hydrogen and phenyl hydrogen-containing silicon oil as matrix, platinum catalyst is curing agent, pass through the synergistic effect between them, obtain novel boryl organosilicon neutron shield composite material, the neutron shield composite material has suitable viscosity and good processability, the new neutron shielding composite has stronger shielding protection effect to neutrons in nuclei and gamma-rays simultaneously, there is good heat-resisting long performance simultaneously, mechanical property and slowing down power(SDP) to fast neutron.
Description
Technical field
The present invention relates to the material shielded to the spentnuclear fuel that nuclear power station generates more particularly to a kind of neutron shielding materials
And preparation method thereof.
Background technique
Neutron is one of the elementary particle of constituting atom core, itself is not charged, but since its speed with higher can make
Substance ionizes, and generates radioactive radiation, is widely used in the fields such as national defence, scientific research, radiotherapy and detection；Neutron exists
Using indispensable in nuclear fission Nuclear Power Development, provide a large amount of clean energy resource for the mankind, however, neutron ionization generate it is big
Amount secondary can interact with histocyte, cause significant damage to human health；Meanwhile neutron irradiation can make in material
Portion generates point defect and dislocation, and material property is made to degenerate, therefore neutrons in nuclei and gamma-ray shielding become new one with protection
For one of the key factor of nuclear energy exploitation.
10B is 3837 targets to the absorption cross-section of thermal neutron, is more than 50 times of NEUTRON PROTECTION material concrete, is to absorb with boron
Boron steel, stereotype and large-sized concrete of main body etc. are used as nuclear defence material of main part, currently on the market the higher paraffin of hydrogen content, poly-
Ethylene etc. becomes preferred nuclear defence high molecular material, however these traditional, single radiation shielding materials have been difficult satisfaction and have answered
With requiring, as lead density is big, and it is toxic, it is mainly used for protecting gamma-rays, but poor to neutron shield effectiveness；Volume of concrete
Greatly and it is difficult to move；The increase of boron aluminium alloy, boron steel, boron content causes material structural strength to decline, and boron content is reduced not
It is able to satisfy performance requirement, the cost for being enriched with boron -10 is very high；The assimilation effect and mechanical property of cadmium stick are fine, but expensive,
It also will form Secondary radiation pollution；Boracic epoxy group shielding material has good heat resistance, but flexible insufficient, is unable to satisfy spy
Different structural shielding requirement；Polyethylene flexible shielding material, which substantially reduces absorption because capturing thermal neutron and releasing secondary gamma-rays, to be hankered
Sub- ability, while it to be first pressed into the plate of certain volume, it is unable to satisfy live encapsulating process for protecting requirement；Therefore, it is badly in need of out
Issuing one kind not only has excellent nuclear defence performance, but also is able to satisfy the neutron shielding material of new construction process requirement, is new core
The basis of energy development and application.
Summary of the invention
In response to the problems existing in the prior art, the purpose of the present invention is to provide a kind of neutron shielding material and its preparation sides
Method.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of neutron shielding material, by weight percentage, including matrix 20-40%, curing agent 20-40%, neutron are inhaled
Receive agent 10-40%, fire retardant 1-5%, densifier 1-5%；Described matrix is by phenyl vinyl polysiloxane, phenyl Silicon Containing Hydrogen
Oil mixes in mass ratio for 1:1-3.
Preferably, the neutron-absorbing material is the boron carbide modified with the aminopropyl triethoxysilane coupling agent surface 3-.
The present invention also provides the neutron-absorbing materials the preparation method is as follows: by 3- aminopropyl triethoxysilane coupling agent
It is by volume that 1:5-10 is mixed with ethyl alcohol, adjustment pH value of solution to 4~5, addition boron carbide ultrasonic disperse is uniform, hydro-thermal at 65 DEG C
4h is reacted, reactant filters, the modified boron carbide in dry the aminopropyl triethoxysilane coupling agent surface 3-；The boron carbide
Solid-to-liquid ratio with overall solution volume is (3-5) mg:1mL；Using nontoxic, "dead", low in cost, high boron content and high temperature resistant
Property boron carbide as neutron absorber material, it is modified to carry out surface to it with 3- aminopropyl triethoxysilane coupling agent, can be with
The interface compatibility for improving boron carbide and phenyl vinyl polysiloxane connects boron carbide in organosilicon even closer and careful,
Improve the neutron shield performance of composite material.
Preferably, the preparation method of the neutron-absorbing material, the drying temperature are 120 DEG C.
Preferably, the curing agent is platinum catalyst；Platinum catalyst can suitably shorten each component gel solidification time, reduce
The sedimentation of solid-state mixture in the liquid state, improves the component uniformity of neutron shielding material.
Preferably, the fire retardant, which is selected from, contains nitrogen expansion type combustion inhibitor, magnesium hydroxide, calcium hydroxide, aluminium hydroxide, boric acid
One of zinc and nickel hydroxide are a variety of；For neutron shielding material of the invention, addition 1-5% fire retardant can reach
Optimal flame retardant property and thermal coefficient.
Preferably, the densifier is selected from tungsten powder, copper powder, iron powder, tungsten oxide, iron oxide, zinc zirconium, zinc powder, oxidation
One of zirconium powder and oxide powder and zinc are a variety of；Densifier can by change content adjust the mixed system uniformity,
Viscosity and solidification process make the viscosity of the system be maintained at appropriate range and avoid being involved in gas during casting, and energy
Solidification temperature and curing time are controlled, the setting rate of the mixed system is accelerated, improves coagulation result, guarantees neutron shielding material
With the excellent performances such as good anti-flammability, thermal conductivity, mechanical property and the stomata of inside be few.
The present invention also provides a kind of preparation methods of neutron shielding material, include the following steps:
S1, phenyl hydrogen-containing silicon oil, phenyl vinyl polysiloxane and curing agent are stirred evenly by the weight percent；
S2, the boron carbide that the weight percent is added stir evenly, and feed the mixture into compacting tool set, and it is de- to carry out vacuum
Bubble processing, is made mixture；
S3, mixture described in step S2 is heating and curing, demolding after cooling.
Preferably, stirring condition is to be stirred to react 0.5-1h at 60-80 DEG C in step S2.
Preferably, condition of cure is 130-160 DEG C of curing reaction 1-3h in the step S3.
Compared with prior art, the beneficial effects of the present invention are:
(1) present invention is using in nontoxic, "dead", low in cost, high boron content and the conduct of the boron carbide of heat-resisting quantity
Sub- absorbing material carries out surface to it with 3- aminopropyl triethoxysilane coupling agent and is modified, improves boron carbide and organosilicon
Interface compatibility problem, all have the compound neutron shield of boryl organosilicon obtained to neutrons in nuclei and gamma-rays simultaneously relatively strong
Shielding protection effect, Secondary radiation will not be caused to pollute.
(2) using the phenyl vinyl polysiloxane of high-content hydrogen and phenyl hydrogen-containing silicon oil as matrix, platinum catalyst is curing agent,
By the synergistic effect between them, make neutron shield composite material obtained that there is suitable viscosity and good mouldability
Can, while there is good heat-resisting long performance, mechanical property and slowing down power(SDP) and lower cubical contraction to fast neutron
To reduce the micro- gas hole defect generated after neutron shielding material cure shrinkage.
Detailed description of the invention
Fig. 1 is the grain size distribution of neutron shielding material made from embodiment 1 and comparative example 1.
Fig. 2 is the cured variable density comparison diagram of neutron shielding material made from embodiment 1 and comparative example 1.
In Fig. 3, (a), (b) are respectively the scanning electron microscope of neutron shielding material made from embodiment 1 and comparative example 1
Phenogram.
Fig. 4 is the infrared spectrum characterization figure of neutron shielding material made from embodiment 1.
In Fig. 5, (a), (b) are respectively the scanning electron microscope after neutron shielding material predose made from embodiment 1
Phenogram；(c), (d) is respectively the scanning electron microscope phenogram after neutron shielding material predose made from comparative example 1.
Fig. 6 is the variable density figure after neutron shielding material predose made from embodiment 2~5.
Fig. 7 is the hot weight curve of neutron shielding material produced by the present invention.
Fig. 8 is the tensile strength figure before and after neutron shielding material sample irradiation made from embodiment 2~5.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated；It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention；Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method
And equipment.
Embodiment 1
A kind of neutron shielding material, by weight percentage, including matrix 30%, platinum catalyst 30%, neutron-absorbing material
30%, nitrogen expansion type combustion inhibitor 5%, tungsten powder 5%；Described matrix presses quality by phenyl vinyl polysiloxane, phenyl hydrogen-containing silicon oil
Than being mixed for 1:2.
The neutron-absorbing material is the boron carbide modified with the aminopropyl triethoxysilane coupling agent surface 3-, preparation side
Method is as follows: with ethyl alcohol being by volume that 1:8 is mixed by 3- aminopropyl triethoxysilane, adjusts pH value of solution to 4~5, according to carbon
The solid-to-liquid ratio for changing boron and overall solution volume is that boron carbide is added in 5mg:1mL and ultrasonic disperse is uniform, and then hydro-thermal is anti-at 65 DEG C
Answer 4h, reactant filters, in 120 DEG C of dry modified boron carbides in the aminopropyl triethoxysilane coupling agent surface 3-.
The preparation method of the neutron shielding material, includes the following steps:
S1, phenyl hydrogen-containing silicon oil, phenyl vinyl polysiloxane and curing agent are stirred evenly by the weight percent；
The modified boron carbide in S2, the aminopropyl triethoxysilane coupling agent surface 3- that the weight percent is added, in 70
It is stirred to react 0.5h at DEG C, feeds the mixture into compacting tool set, carries out vacuum defoamation processing, mixture is made；
S3, be heating and curing mixture described in step S2 2h at 140 DEG C, demolding after cooling.
Embodiment 2
The present embodiment provides a kind of neutron shielding materials, by weight percentage, including matrix 40%, platinum catalyst
20%, neutron-absorbing material 30%, magnesium hydroxide 5%, zinc powder 5%；Described matrix is by phenyl vinyl polysiloxane, phenyl Silicon Containing Hydrogen
Oil mixes in mass ratio for 1:1.
The neutron-absorbing material is the boron carbide modified with the aminopropyl triethoxysilane coupling agent surface 3-, preparation side
Method is as follows: with ethyl alcohol being by volume that 1:5 is mixed by 3- aminopropyl triethoxysilane, adjusts pH value of solution to 4~5, according to carbon
The solid-to-liquid ratio for changing boron and overall solution volume is that boron carbide is added in 3mg:1mL and ultrasonic disperse is uniform, and then hydro-thermal is anti-at 65 DEG C
Answer 4h, reactant filters, in 120 DEG C of dry modified boron carbides in the aminopropyl triethoxysilane coupling agent surface 3-.
The preparation method of the neutron shielding material, includes the following steps:
S1, phenyl hydrogen-containing silicon oil, phenyl vinyl polysiloxane and curing agent are stirred evenly by the weight percent；
The modified boron carbide in S2, the aminopropyl triethoxysilane coupling agent surface 3- that the weight percent is added, in 60
It is stirred to react 1h at DEG C, feeds the mixture into compacting tool set, carries out vacuum defoamation processing, mixture is made；
S3, be heating and curing mixture described in step S2 1h at 130 DEG C, demolding after cooling.
Embodiment 3
The present embodiment provides a kind of neutron shielding materials, by weight percentage, including matrix 40%, platinum catalyst
20%, neutron-absorbing material 38%, calcium hydroxide 1%, tungsten oxide 1%；Described matrix is hydrogeneous by phenyl vinyl polysiloxane, phenyl
Silicone oil mixes in mass ratio for 1:3.
The neutron-absorbing material is the boron carbide modified with the aminopropyl triethoxysilane coupling agent surface 3-, preparation side
Method is as follows: with ethyl alcohol being by volume that 1:10 is mixed by 3- aminopropyl triethoxysilane, adjusts pH value of solution to 4~5, according to carbon
The solid-to-liquid ratio for changing boron and overall solution volume is that boron carbide is added in 5mg:1mL and ultrasonic disperse is uniform, and then hydro-thermal is anti-at 65 DEG C
Answer 4h, reactant filters, in 120 DEG C of dry modified boron carbides in the aminopropyl triethoxysilane coupling agent surface 3-.
The preparation method of the neutron shielding material, includes the following steps:
S1, phenyl hydrogen-containing silicon oil, phenyl vinyl polysiloxane and curing agent are stirred evenly by the weight percent；
The modified boron carbide in S2, the aminopropyl triethoxysilane coupling agent surface 3- that the weight percent is added, in 80
It is stirred to react 0.5h at DEG C, feeds the mixture into compacting tool set, carries out vacuum defoamation processing, mixture is made；
S3, be heating and curing mixture described in step S2 3h at 160 DEG C, demolding after cooling.
Embodiment 4
The present embodiment provides a kind of neutron shielding materials, and by weight percentage, compared with embodiment 1, difference exists
In, including matrix 40%, platinum catalyst 40%, neutron-absorbing material 10%, zinc borate 5%, zinc zirconium 5%.
Remaining is same as Example 1.
Embodiment 5
The present embodiment provides a kind of neutron shielding materials, and by weight percentage, compared with embodiment 1, difference exists
In, including matrix 40%, platinum catalyst 36%, neutron-absorbing material 20%, zinc borate 2%, zinc zirconium 2%.
Remaining is same as Example 1.
Embodiment 6
The present embodiment provides a kind of neutron shielding materials, compared with Example 1, the difference is that, the fire retardant is
Aluminium hydroxide is mixed with nickel hydroxide 1:1 in mass ratio.
Remaining is identical in embodiment 1.
Embodiment 7
The present embodiment provides a kind of neutron shielding materials, compared with Example 1, the difference is that, the density increases
Agent is mixed in mass ratio for 1:5 by iron oxide with zirconia powder.
Remaining is identical in embodiment 1.
Comparative example 1
This comparative example provides a kind of neutron shielding material, compared with Example 1, the difference is that, the neutron-absorbing
Agent is boron carbide, modified without the aminopropyl triethoxysilane coupling agent surface 3-.
Remaining is all the same with embodiment 1.
Comparative example 2
This comparative example provides a kind of neutron shielding material, compared with Example 1, the difference is that, described matrix is by benzene
Base vinyl polysiloxane, phenyl hydrogen-containing silicon oil mix in mass ratio for 1:0.5.
Remaining is all the same with embodiment 1.
Comparative example 3
This comparative example provides a kind of neutron shielding material, compared with Example 1, the difference is that, the neutron-absorbing
Agent the preparation method is as follows: with ethyl alcohol be by volume that 1:3 is mixed by 3- aminopropyl triethoxysilane coupling agent, adjust solution
PH to 4~5, is added that boron carbide ultrasonic disperse is uniform, and hydro-thermal reaction 4h at 65 DEG C, reactant filters, dry 3- aminopropyl three
The modified boron carbide in Ethoxysilane coupling agent surface；The solid-to-liquid ratio of the boron carbide and overall solution volume is 5mg:1mL.
Remaining is all the same with embodiment 1.
Comparative example 4
This comparative example provides a kind of neutron shielding material, compared with Example 1, the difference is that, the neutron-absorbing
In the preparation method of agent, hydrothermal temperature is 80 DEG C.
Remaining is all the same with embodiment 1.
Comparative example 5
This comparative example provides a kind of neutron shielding material, compared with Example 1, the difference is that, the neutron-absorbing
In the preparation method of agent, the solid-to-liquid ratio of the boron carbide and overall solution volume is 2mg:1mL.
Remaining is all the same with embodiment 1.
Application examples 1
Embodiment 1 and the partial size of neutron shielding material made from comparative example 1 are analyzed, as a result as shown in Figure 1, by scheming
Middle result is it is found that average grain of the embodiment 1 through the modified neutron shielding material in the aminopropyl triethoxysilane coupling agent surface 3-
Shown in diameter such as Fig. 1 (a), about 680nm, compared with the 1 small about 200- of unmodified neutron shielding material Fig. 1 (b) average grain diameter of comparative example
300nm, this is because 3- aminopropyl triethoxysilane forms one layer of organic film, interparticle steric hindrance in carbonization boron surface
Enhancing, so that not easy to reunite between particle, partial size accordingly also becomes smaller, and polydispersity coefficient accordingly reduces.
After neutron shielding material curing molding made from embodiment 1 and comparative example 1, every 20mm cuts one section, measures close
Degree, as a result as shown in Fig. 2, as result in figure it is found that the variable density of neutron shield composite material made from embodiment 1 is smaller,
The variable density amplitude of neutron shield composite material made from comparative example 1 is larger, illustrates that neutron shield made from embodiment 1 is compound
Material is since to carbonization boron modification, anti-settling effect is unmodified compared with comparative example 1 good；This is because modified carbonization boron surface packet
Covering after one layer of KH550 film has good compatibility with matrix organosilicon, in forming composite material, organic and inorganic interface
Effect enhancing, connects closer and more evenly.
Neutron shielding material made from embodiment 1 and comparative example 1 is scanned electron microscope characterization, as a result respectively such as
In (a) in Fig. 3, Fig. 3 shown in (b), by result in figure it is found that the carbon coupling agent modified without 3- aminopropyl triethoxysilane
It is irregular to change the distribution of neutron shielding material made from boron, easily reunites, is not easy to reach good dispersion effect in matrix organosilicon
Fruit；And passes through neutron shielding material distribution made from the coupling agent modified boron carbide of 3- aminopropyl triethoxysilane and compare rule
It is whole, it is uniformly distributed loosely and at random；This is because being made by the coupling agent modified boron carbide of 3- aminopropyl triethoxysilane
Neutron shielding material surface grafting on organic group, increase interparticle steric hindrance, it is not easy to reunite.
Neutron shielding material made from embodiment 1 is subjected to infrared spectrum characterization, as a result as shown in Fig. 4, embodiment 1 is passed through
Cross neutron shielding material made from the coupling agent modified boron carbide of 3- aminopropyl triethoxysilane, 3434cm-1The peak-OH at place is bright
It is aobvious to weaken, and 2918cm-1, 2851cm-1It is the overlapped knot of antisymmetric stretching vibration absorption band of methyl, methylene
Fruit, 1085cm-1The characteristic spikes at place are that B-C key and Si-O key are overlapped as a result, 1554cm in boron carbide-1The width at place
Peak is N-H overlapping as a result, result has sufficiently shown on neutron shielding material surface grafting 3- aminopropyl triethoxysilane, is changed
The surface nature for having become filler facilitates the interface compatibility of enhancing with matrix.
Scanning electron microscope characterization, knot will be carried out after neutron shielding material predose made from embodiment 1 and comparative example 1
Fruit is as shown in figure 5, the scanning electron microscope phenogram after neutron shielding material predose, irradiation made from embodiment 1 is distinguished
In Fig. 5 (a), in Fig. 5 shown in (b)；Scanning electron microscopy after neutron shielding material predose, irradiation made from comparative example 1
Mirror phenogram is respectively as shown in (d) in (c) in Fig. 5, Fig. 5, and wherein irradiation dose is 1000kGy, by result in Fig. 5 it is found that not
By neutron shielding material boron carbide particles made from the coupling agent modified boron carbide of 3- aminopropyl triethoxysilane compound
It is unevenly distributed in material, Yi Fasheng agglomeration, forms defect, to influence the mechanical property of composite material, and pass through 3-
Neutron shielding material made from the coupling agent modified boron carbide of aminopropyl triethoxysilane has preferable in organic silicon substrate
Dispersion effect, surface is smooth, agglomeration be improved significantly, interface cohesion is preferable, this is because modified carbonization boron surface
It has connected organic group and partial size is more unmodified small, increased interparticle steric hindrance, so that it is not easy to reunite between particle,
The interface cohesion of composite material is more preferable after irradiation.
Application examples 2
Variable density after neutron shielding material predose made from embodiment 2~5 is detected, neutron shielding material
Variable density after predose as shown in fig. 6, by figure it is found that with neutron-absorbing material mass fraction increase, it is obtained in
The variable density value of sub- shielding material is gradually increased, this is because the addition of neutron-absorbing material improves the cause of neutron shielding material
Density, neutron shielding material is by irradiation, and density becomes larger, and irradiation dose is bigger, and variable density is bigger, this is because high energy spoke
It penetrates to cause and forms cross-linked network between polymeric chain, density is made to become larger.
Application examples 3
For the heat resistance for studying neutron shielding material produced by the present invention, embodiment 1, embodiment 4, embodiment are tested
5 and comparative example 1 made from neutron shielding material from the thermogravimetric curve under the conditions of room temperature~840 DEG C, as a result as shown in Figure 7；With Ts
As the initial temperature that material decomposes, table 1 lists material and decomposes 5% temperature (T5d), decomposes 10% temperature (T10d) and 840
DEG C when carbon yield (Ycat840℃)。
| T5d/℃ | T10d/℃ | YCat840 DEG C/% | |
| Embodiment 1 | 620 | 638 | 80.2 |
| Embodiment 4 | 595 | 612 | 72.9 |
| Embodiment 5 | 605 | 625 | 76.8 |
| Comparative example 1 | 540 | 565 | 59.1 |
In conjunction with Fig. 7 and 1 interpretation of result of table it is found that the boron carbide system coupling agent modified by 3- aminopropyl triethoxysilane
The heat resistance of the neutron shielding material obtained has to be improved by a relatively large margin, and with the increase of neutron-absorbing agent content, neutron screen
The heat resistance for covering material further increases, and carbon yield is also in rising trend under hot conditions, illustrates through three ethoxy of 3- aminopropyl
The coupling agent modified boron carbide of base silane can significantly improve the heat resistance of neutron shielding material, to make in produced by the present invention
The thermal decomposition temperature of sub- shielding material improves.
Application examples 4
As by before and after neutron shielding material sample irradiation made from embodiment 2~5 with certain loading speed ((1 ±
0.5) mm/min) under the conditions of tensile strength carry out material mechanical property characterization, as a result as shown in Figure 8；As shown in Figure 8, with
The tensile strength of the increase of boron carbide mass fraction, composite material gradually increases, this is because modified neutron-absorbing material surface connects
Organic group is gone up, it is easier to be evenly dispersed in matrix organosilicon, while partial size is more unmodified small, partial size small specific surface
Product is big, and the chance for adsorbing macromolecular chain is more, the Interaction enhanced with matrix organosilicon, thus to the power of neutron shielding material
Learning performance has facilitation；By irradiation, tensile strength has small size increase, and irradiation dose is bigger, and tensile strength is bigger, this is
Due to forming cross-linked network between radiation-initiated polymerization object macromolecular chain, mechanical property is improved.
Application examples 5
For high temperature resistant type thermoneutron radiation shielding properties research still in its infancy, the thermal neutron shielding of material
Can be the closest with the relation with contents of neutron absorber material, the present invention using CMR cold neutrons photographic means determine embodiment 1~
7 and comparative example 1~5 under the conditions of neutron shielding material thermoneutron radiation shielding properties, wherein neutron transmission rate I/I.For table
The ratio that neutron penetrates shielding material is levied, wherein I is the intensity value that neutron penetrates shielding material, I.Reference material is penetrated for neutron
Intensity value, measurement result is as shown in the table.
As result in table it is found that neutron shielding material made from the embodiment of the present invention 1~7 is with neutron-absorbing agent content
Increase, neutron shielding material shows preferable thermal neutron shielding properties and increases, and neutron shielding material made from comparative example
Thermal neutron shielding properties weakens, illustrate the present invention mutually cooperateed with as each component make made from neutron shielding material with stronger
Neutron shield efficiency, and change either condition, neutron shielding material performance can all be had an impact；Pass through embodiment 1 and comparison
1 result of example is compared, and illustrates that neutron can be significantly improved to carbonization boron modification by 3- aminopropyl triethoxysilane coupling agent
The shielding properties of shielding material.
The above, only of the invention illustrates embodiment, not to the present invention in any form with substantial limitation,
It should be pointed out that for those skilled in the art, under the premise of not departing from the method for the present invention, that makes several changes
It also should be regarded as protection scope of the present invention into supplement；All those skilled in the art, do not depart from spirit of that invention and
In the case where range, using the equivalent variations of a little change, modification and differentiation that disclosed above technology contents are made, it is
Equivalent embodiment of the invention；Meanwhile any equivalent variations that all substantial technologicals according to the present invention do above-described embodiment
Change, modification and differentiation, still fall within protection scope of the present invention.
Claims (10)
1. a kind of neutron shielding material, which is characterized in that by weight percentage, including matrix 20-40%, curing agent 20-40%,
Neutron-absorbing material 10-40%, fire retardant 1-5%, densifier 1-5%；Described matrix is contained by phenyl vinyl polysiloxane, phenyl
Hydrogen silicone oil mixes in mass ratio for 1:1-3.
2. a kind of neutron shielding material according to claim 1, which is characterized in that the neutron-absorbing material is with 3- ammonia third
The modified boron carbide in ethyl triethoxy silicane alkane coupling agent surface.
3. a kind of neutron shielding material according to claim 1 or 2, which is characterized in that the preparation of the neutron-absorbing material
Method is as follows: it with ethyl alcohol is by volume that 1:5-10 is mixed by 3- aminopropyl triethoxysilane coupling agent, adjustment pH value of solution to 4
~ 5, it is added that boron carbide ultrasonic disperse is uniform, and hydro-thermal reaction 4h at 65 DEG C, reactant filters, dry 3- aminopropyl-triethoxy
The modified boron carbide in silane coupling agent surface；The solid-to-liquid ratio of the boron carbide and overall solution volume is (3-5) mg:1mL.
4. a kind of neutron shielding material according to claim 3, which is characterized in that the drying temperature is 120 DEG C.
5. a kind of neutron shielding material according to claim 1 or 2, which is characterized in that the curing agent is platinum catalyst.
6. a kind of neutron shielding material according to claim 1, which is characterized in that the fire retardant, which is selected from, contains nitrogen expansion type
One of fire retardant, magnesium hydroxide, calcium hydroxide, aluminium hydroxide, zinc borate and nickel hydroxide are a variety of.
7. a kind of neutron shielding material according to claim 1, which is characterized in that the densifier be selected from tungsten powder,
One of copper powder, iron powder, tungsten oxide, iron oxide, zinc zirconium, zinc powder, zirconia powder and oxide powder and zinc are a variety of.
8. a kind of preparation method of neutron shielding material described in claim 1, which comprises the steps of:
S1, phenyl hydrogen-containing silicon oil, phenyl vinyl polysiloxane, fire retardant and curing agent are stirred by the weight percent
It is even；
S2, sequentially add the neutron-absorbing material of the weight percent into step S1, densifier stirs evenly, will mix
Object is added in compacting tool set, carries out vacuum defoamation processing, and mixture is made；
S3, mixture described in step S2 is heating and curing, demolding after cooling.
9. a kind of preparation method of neutron shielding material according to claim 1, which is characterized in that stirring bar in step S2
Part is to be stirred to react 0.5-1h at 60-80 DEG C.
10. a kind of preparation method of neutron shielding material according to claim 1, which is characterized in that solidify in step S3
Condition is 130-160 DEG C of curing reaction 1-3h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111489796A (en) * | 2020-03-24 | 2020-08-04 | 上海交通大学 | Method, system and medium for calculating neutron shielding performance of material |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710727A (en) * | 2015-03-27 | 2015-06-17 | 中国科学院长春应用化学研究所 | Epoxy resin based neutron and gamma ray shielding composite material, as well as preparation method and application thereof |
| CN107189419A (en) * | 2017-05-26 | 2017-09-22 | 东莞市奥能工程塑料有限公司 | A kind of ultralow-hydrogen low anti-neutron irradiation material and preparation method thereof |
| CN107955332A (en) * | 2017-12-04 | 2018-04-24 | 北京航空航天大学 | A kind of neutron shield superhybrid composite laminate and preparation method thereof |
| CN108335771A (en) * | 2017-12-26 | 2018-07-27 | 中广核研究院有限公司 | Neutron shielding material and preparation method thereof |
| CN108659469A (en) * | 2018-05-18 | 2018-10-16 | 北京市射线应用研究中心 | The epoxy resin-matrix neutron shielding material and preparation and application that organic siliconresin is modified |
| CN109192348A (en) * | 2018-07-04 | 2019-01-11 | 北京市射线应用研究中心 | One kind can pour type silicon rubber base heatproof shielding material and preparation method thereof |
-
2019
- 2019-01-16 CN CN201811338119.4A patent/CN109575606A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710727A (en) * | 2015-03-27 | 2015-06-17 | 中国科学院长春应用化学研究所 | Epoxy resin based neutron and gamma ray shielding composite material, as well as preparation method and application thereof |
| CN107189419A (en) * | 2017-05-26 | 2017-09-22 | 东莞市奥能工程塑料有限公司 | A kind of ultralow-hydrogen low anti-neutron irradiation material and preparation method thereof |
| CN107955332A (en) * | 2017-12-04 | 2018-04-24 | 北京航空航天大学 | A kind of neutron shield superhybrid composite laminate and preparation method thereof |
| CN108335771A (en) * | 2017-12-26 | 2018-07-27 | 中广核研究院有限公司 | Neutron shielding material and preparation method thereof |
| CN108659469A (en) * | 2018-05-18 | 2018-10-16 | 北京市射线应用研究中心 | The epoxy resin-matrix neutron shielding material and preparation and application that organic siliconresin is modified |
| CN109192348A (en) * | 2018-07-04 | 2019-01-11 | 北京市射线应用研究中心 | One kind can pour type silicon rubber base heatproof shielding material and preparation method thereof |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111489796B (en) * | 2020-03-24 | 2022-06-10 | 上海交通大学 | Method, system and medium for calculating neutron shielding performance of material |
| CN111489796A (en) * | 2020-03-24 | 2020-08-04 | 上海交通大学 | Method, system and medium for calculating neutron shielding performance of material |
| CN111933322A (en) * | 2020-08-13 | 2020-11-13 | 中国核动力研究设计院 | High-temperature-resistant neutron shielding assembly and preparation method thereof |
| CN112500706A (en) * | 2020-11-23 | 2021-03-16 | 中广核高新核材科技（苏州）有限公司 | Neutron shielding fireproof silicone adhesive and preparation method thereof |
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| CN113201180A (en) * | 2021-05-13 | 2021-08-03 | 中国科学院合肥物质科学研究院 | Neutron and gamma ray composite shielding material and preparation method thereof |
| CN113201180B (en) * | 2021-05-13 | 2024-03-01 | 中国科学院合肥物质科学研究院 | Neutron and gamma ray composite shielding material and preparation method thereof |
| CN113604054A (en) * | 2021-08-09 | 2021-11-05 | 中国工程物理研究院化工材料研究所 | Castable temperature-resistant boron-containing neutron shielding absorption material and preparation process thereof |
| CN113563724A (en) * | 2021-08-09 | 2021-10-29 | 中国工程物理研究院化工材料研究所 | Organosilicon composite material with neutron shielding efficiency and heat insulation efficiency and preparation process thereof |
| CN113773651A (en) * | 2021-09-02 | 2021-12-10 | 中海油常州涂料化工研究院有限公司 | Normal-temperature cured neutron shielding material and preparation method thereof |
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