CN108257702B - Hydrogen-free neutron shielding material of a kind of high intensity high boron content and preparation method thereof - Google Patents

Hydrogen-free neutron shielding material of a kind of high intensity high boron content and preparation method thereof Download PDF

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Publication number
CN108257702B
CN108257702B CN201810051927.6A CN201810051927A CN108257702B CN 108257702 B CN108257702 B CN 108257702B CN 201810051927 A CN201810051927 A CN 201810051927A CN 108257702 B CN108257702 B CN 108257702B
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shielding material
neutron shielding
hydrogen
boron content
boron
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CN108257702A (en
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邱永福
常学义
程志毓
范洪波
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Dongguan University of Technology
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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
    • G21F1/02—Selection of uniform shielding materials
    • G21F1/06—Ceramics; Glasses; Refractories
    • 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

Abstract

The present invention provides hydrogen-free neutron shielding material of a kind of high-intensitive high boron content and preparation method thereof, wherein the preparation method comprises the following steps: being ground to powder after 1 ~ 4 part of silica, 1 ~ 5 part of aluminum oxide, 3 ~ 8 parts of potassium phosphates, 1 ~ 4 part of diboron trioxide and 0.2 ~ 1.5 part of calcium oxide are mixed, it is uniformly mixed with 80 ~ 90 parts of boron carbide powders, compression moulding, in 500 ~ 550 DEG C of air atmosphere low temperature sinterings, the neutron shielding material that boron content is 63 ~ 71 wt% is obtained.It is uniformly mixed due to being added in boron carbide using silica, aluminum oxide, potassium phosphate, diboron trioxide and the calcium oxide of aforementioned proportion mixing as sintering aid, only need 500 ~ 550 DEG C temperature condition and carry out in air atmosphere low-temperature sintering, simplify existing preparation process, and above-mentioned sintering aid can wrap up boron carbide-based body at the process conditions and form very fine and close radiation protective layer, and the high boron of neutron shielding material is hydrogen-free and has high-intensity performance.

Description

Hydrogen-free neutron shielding material of a kind of high intensity high boron content and preparation method thereof
Technical field
The present invention relates to neutron shielding material fields, and in particular to a kind of hydrogen-free neutron shielding material of high intensity high boron content And preparation method thereof.
Background technique
With atomic energy industry, Radiation Medicine and the rapid development of national defence scientific research, the research of middle subdomains is also continuous deep Enter.Due to the stronger feature of the penetration power of neutron, it is easy to generate periphery object and personnel irradiation damage, therefore core screen must be utilized It covers material to shield neutron, prevents from damaging people.
Neutron shielding material is divided to Moderation of the fast neutrons and slow neutron to absorb two kinds the effect of neutron shield.Moderation of the fast neutrons is Refer to that inelastic scattering occurs for the heavy nucleus element such as fast neutron and iron, tungsten, or with after the light nucleus element generation elastic scattering such as hydrogen, fast neutron Energy by scattering loss, to be changed into slow neutron.Slow neutron absorbs the compound for referring to boron, lithium, part rare earth element etc. With larger slow neutron absorption cross-section, can be very good to absorb slow neutron, especially containing the material of boron element, such as boron carbide (B4It C) is the most common neutron absorber, with cheap, slow neutron absorption cross-section is big, processing and forming is more convenient, hot steady There is no stronger gamma-rays secondary radiation after qualitative good, absorption neutron, is easy to the advantages that protecting, B4C is used as neutron screen extensively Cover material function filler.
In recent years, for development structure/function integration neutron shielding material demand, some grind has been carried out both at home and abroad Study carefully, such as lead-boron polythene, glass fibre (or carbon fiber)/epoxy resin/B4C composite, BN/ high density polyethylene (HDPE) composite wood Material, B4C/SEBS thermoplastic elastomer composite material, B4C/SBR composite material etc. is for the device that structure is complicated or position is special Part surface carries out the flexible neutron shielding material of package shielding and military-civil NEUTRON PROTECTION clothes；In addition such as boronated stainless steel, hydrogen Boronation pick/hydrogenation pick, B4The neutron shielding material for engineering structure of a batch high-strength and high-modulus such as C/Al.
Although there is the research of some neutron shielding materials both at home and abroad at present, due to usual high temperature in a vacuum or inert atmosphere Neutron shielding material is prepared in sintering, and the process conditions are more demanding to the condition of temperature, and hot conditions can expend largely The energy；Simultaneously because needing to be arranged vacuum or inert atmosphere, it just can ensure that boron carbide keeps superperformance, further limit system Standby process conditions, increase preparation process difficulty.B4The sintering B that C fusing point is high and hardness is big, pure4C is difficult machine-shaping, and It is expensive.How to make neutron shielding material keep high boron and without under the premise of protium, reduces sintering temperature and broadening Fabrication process condition becomes the critical issue that industry needs to solve.
Summary of the invention
To solve the above problems, the application provides a kind of hydrogen-free neutron shielding material of high-intensitive high boron content and its preparation side Method, the neutron shielding material have the characteristics that mechanical strength is high, while having the advantages that preparation process is simple and manufacturing cost is lower.
According in a first aspect, providing a kind of high-intensitive hydrogen-free neutron shielding material of high boron content, shielding in a kind of embodiment Material includes following components:
1 ~ 4 part of silica；
1 ~ 5 part of aluminum oxide；
3 ~ 8 parts of potassium phosphates；
1 ~ 4 part of diboron trioxide；
0.2 ~ 1.5 part of calcium oxide, and
80 ~ 90 parts of boron carbides；
Boron content in neutron shielding material is 63 ~ 71 wt%.
Further, the density of neutron shielding material is 1.6 ~ 1.8 g/cm3。
Further, the compression strength of neutron shielding material is 29 ~ 65MPa.
According to second aspect, is provided in a kind of embodiment and a kind of prepare the hydrogen-free neutron shield material of above-mentioned high-intensitive high boron content The method of material, will
1 ~ 4 part of silica；
1 ~ 5 part of aluminum oxide；
3 ~ 8 parts of potassium phosphates；
1 ~ 4 part of diboron trioxide；And
0.2 ~ 1.5 part of calcium oxide is ground to powder after being mixed, and is uniformly mixed with 80 ~ 90 parts of boron carbide powders, compacting Molding obtains the neutron shielding material that boron content is 63 ~ 71 wt% in 500 ~ 550 DEG C of air atmosphere low temperature sinterings.The neutron The density of shielding material is 1.6 ~ 1.8 g/cm3, the compression strength of neutron shielding material is 29 ~ 65MPa.
Further, silica, aluminum oxide, potassium phosphate, diboron trioxide and calcium oxide are ground to average grain diameter For 1 ~ 5 micron of powder.
Further, boron carbide powder was the boron carbide micro powder that partial size is micron after 150 ~ 800 meshes.
Further, the pressure applied in compression moulding is 10 ~ 25 MPa.
Further, the temperature of air atmosphere low temperature sintering is 510 ~ 540 DEG C.
According to the hydrogen-free neutron shielding material of high-intensitive high boron content of above-described embodiment, due to using aforementioned proportion mixing Silica, aluminum oxide, potassium phosphate, diboron trioxide and calcium oxide are added in boron carbide as sintering aid and carry out Even mixing, it is only necessary to carry out low-temperature sintering in 500 ~ 550 DEG C of temperature conditions and in air atmosphere, simplify existing system Standby technique, and above-mentioned sintering aid can wrap up boron carbide-based body at the process conditions and form very fine and close radiation protection Layer, the high boron of neutron shielding material is hydrogen-free and has high-intensity performance.
Detailed description of the invention
Fig. 1 is the process of the preparation method of the hydrogen-free neutron shielding material of high-intensitive high boron content in an embodiment of the present invention Figure；
Fig. 2 is TG figure of the NSM sample in dry air in an embodiment of the present invention；
Fig. 3 is the scanning electron microscope (SEM) photograph of the NSM sample in an embodiment of the present invention；
Fig. 4 is the resistance to compression curve graph of the NSM sample in the embodiment of the present invention one；
Fig. 5 is the resistance to compression curve graph of the NSM sample in the embodiment of the present invention three.
Specific embodiment
Below by specific embodiment combination attached drawing, invention is further described in detail.
Each step that method describes in specification can also according to those skilled in the art institute can obvious mode into Row sequence is exchanged or adjustment.
One embodiment of the invention provides a kind of high-intensitive high boron content hydrogen-free neutron shielding material, and neutron shielding material includes Following components:
1 ~ 4 part of silica；
1 ~ 5 part of aluminum oxide；
3 ~ 8 parts of potassium phosphates；
1 ~ 4 part of diboron trioxide；
0.2 ~ 1.5 part of calcium oxide, and
80 ~ 90 parts of boron carbides；
Boron content in neutron shielding material is 63 ~ 71 wt%, and density is 1.6 ~ 1.8 g/cm3, compression strength is 29~65MPa。
Boron has many advantages, such as very big neutron absorption cross-section, resourceful, cheap, is ideal neutron-absorbing Element.And B4C is boron content highest and stable compound other than boron simple substance, therefore as neutron-absorbing screen of the invention The matrix of material is covered, and uses silica, aluminum oxide, potassium phosphate, diboron trioxide and the oxidation of aforementioned proportion mixing Calcium is as sintering aid, the high inorganic bond object of intensity easy to form at low temperature.Therefore after low-temperature sintering, sintering aid energy Enough package boron carbide forms very fine and close radiation protective layer, the effect of enhancing shielding neutron.
Referring to Figure 1, the present embodiment, which also provides, a kind of prepares the above-mentioned high-intensitive hydrogen-free neutron shielding material of high boron content Method, specific steps include:
S1, mixed sintering auxiliary agent: by 1 ~ 4 part of silica, 1 ~ 5 part of aluminum oxide, 3 ~ 8 parts of potassium phosphates, 1 ~ 4 part Diboron trioxide and 0.2 ~ 1.5 part of calcium oxide are uniformly mixed；
S2, grinding and sintering auxiliary agent: the mixture that S1 is obtained is added in nanon ball-mill, and dry ball milling to average grain diameter is 1 ~ 5 micron of powder；
S3, raw material mixing, compression moulding: powder obtained in S2 are uniformly mixed with 80 ~ 90 parts of boron carbide powders, with pressure The compression moulding under the pressure of 10 ~ 25 MPa of power machine, wherein boron carbide powder was the carbon that partial size is micron after 150 ~ 800 meshes Change boron micro mist.Sintering aid and boron carbide are ground to the micro mist that average grain diameter is micron, and reason is that partial size is smaller, are sintered Auxiliary agent and boron carbide more uniform can mix, and partial size is smaller, and the shielding material intensity being sintered out is higher.If partial size is big The shielding material intensity obtained after above range, sintering is lower, and using effect should be obtained by being not achieved, and receives if partial size reaches The mixing of meter level, sintering aid and boron carbide can be more uniform, and the performance of shielding material can be more preferable after sintering, but preparation process Complexity, and higher cost.
S4, low-temperature sintering: low-temperature sintering is carried out to the mixture that S3 is obtained in 500 ~ 550 DEG C of air atmospheres, obtains boron Content is 63 ~ 71 wt%, and density is 1.6 ~ 1.8 g/cm3, compression strength is during the high-intensitive high boron content of 29 ~ 65MPa is hydrogen-free Sub- shielding material (NSM).
Refer to Fig. 2, Fig. 2 is thermogravimetric curve of the NSM sample in air atmosphere that boron content is 63%, it can be seen that multiple Condensation material is all highly stable at 600 DEG C or less, and 643 DEG C or more NSM samples start to aoxidize in air, and product starts to increase weight, and puts Heat out.
The main reason for discovery water absorbing properties are deteriorated under study for action as a result, is due to 600 DEG C or more B4C, which is oxidized, to be caused. If carrying out high temperature sintering to shielding material in air atmosphere, shielding material is easily oxidized in sintering process, water imbibition It is deteriorated.Existing preparation process uses high temperature sintering technique under high-temperature vacuum sintering technology or inert atmosphere mostly, thus It can avoid shielding material oxidation, to improve the performance of shielding material.But existing preparation process is more complex, process conditions are tight Lattice, often will cause that yield rate is lower and the higher problem of preparation cost.The present invention avoids B by using low-temperature sintering4C exists It is oxidized in air atmosphere, solves B in air atmosphere4C sintered body is easy the problem of water suction causes performance to decline.
Fig. 3 is referred to, by the structure of scanning electron microscopic observation NSM sample, although the content of boron carbide is up to 80 ~ 90 Wt%, but boron carbide micro powder 1 disperses highly uniform, and boron carbide micro powder 1 is sintered auxiliary agent 2 and is wrapped to form very fine and close radiation protection Layer, without obvious hole.
Embodiment one
In the present embodiment, provide a kind of high-intensitive high boron content hydrogen-free neutron shielding material, neutron shielding material includes Following components:
1 part of silica；
1 part of aluminum oxide；
3 parts of potassium phosphates；
1 part of diboron trioxide；
0.2 part of calcium oxide, and
80 parts of boron carbides；
Boron content in shielding material is 63 ~ 71 wt%, and density is 1.6 ~ 1.8 g/cm3, compression strength be 29 ~ 65MPa。
The present embodiment also provides a kind of method for preparing the hydrogen-free neutron shielding material of above-mentioned high-intensitive high boron content, specific to walk Suddenly include:
S1, mixed sintering auxiliary agent: by 1 part of silica, 1 part of aluminum oxide, 3 parts of potassium phosphates, 1 part of diboron trioxide and 0.2 part of calcium oxide is uniformly mixed；
S2, grinding and sintering auxiliary agent: the mixture that S1 is obtained is added in nanon ball-mill, and dry ball milling to average grain diameter is 1 micron of powder；
S3, raw material mixing, compression moulding: powder obtained in S2 is uniformly mixed with 80 parts of boron carbide powders, uses pressure Machine compression moulding under the pressure of 10 MPa, wherein boron carbide powder was the boron carbide that partial size is micron after 150 ~ 800 meshes Micro mist.
S4, low-temperature sintering: low-temperature sintering is carried out to the mixture that S3 is obtained in 500 DEG C of air atmospheres, obtains boron content For 63 ~ 71 wt%, density is 1.6 ~ 1.8 g/cm3, compression strength is the hydrogen-free neutron screen of high-intensitive high boron content of 29 ~ 65MPa Cover material.
Embodiment two
In the present embodiment, provide a kind of high-intensitive high boron content hydrogen-free neutron shielding material, neutron shielding material includes Following components:
2 parts of silica；
3 parts of aluminum oxides；
5 parts of potassium phosphates；
2 parts of diboron trioxides；
1 part of calcium oxide, and
85 parts of boron carbides；
Boron content in neutron shielding material is 63 ~ 71 wt%, and density is 1.6 ~ 1.8 g/cm3, compression strength is 29~65MPa。
The present embodiment also provides a kind of method for preparing the hydrogen-free neutron shielding material of above-mentioned high-intensitive high boron content, specific to walk Suddenly include:
S1, mixed sintering auxiliary agent: by 2 parts of silica, 3 parts of aluminum oxides, 5 parts of potassium phosphates, 2 parts of diboron trioxides and 1 part of calcium oxide is uniformly mixed；
S2, grinding and sintering auxiliary agent: the mixture that S1 is obtained is added in nanon ball-mill, and dry ball milling to average grain diameter is 1 micron of powder；
S3, raw material mixing, compression moulding: powder obtained in S2 is uniformly mixed with 85 parts of boron carbide powders, uses pressure Machine compression moulding under the pressure of 20 MPa, wherein boron carbide powder was the boron carbide that partial size is micron after 150 ~ 800 meshes Micro mist.
S4, low-temperature sintering: low-temperature sintering is carried out to the mixture that S3 is obtained in 530 DEG C of air atmospheres, obtains boron content For 63 ~ 71 wt%, density is 1.6 ~ 1.8 g/cm3, compression strength is the hydrogen-free neutron screen of high-intensitive high boron content of 29 ~ 65MPa Cover material.
Embodiment three
In the present embodiment, provide a kind of high-intensitive high boron content hydrogen-free neutron shielding material, shielding material includes following Component:
4 parts of silica；
5 parts of aluminum oxides；
8 parts of potassium phosphates；
4 parts of diboron trioxides；
1.5 parts of calcium oxide, and
90 parts of boron carbides；
Boron content in shielding material is 63 ~ 71 wt%, and density is 1.6 ~ 1.8 g/cm3, compression strength be 29 ~ 65MPa。
The present embodiment also provides a kind of method for preparing the hydrogen-free neutron shielding material of above-mentioned high-intensitive high boron content, specific to walk Suddenly include:
S1, mixed sintering auxiliary agent: by 4 parts of silica, 5 parts of aluminum oxides, 8 parts of potassium phosphates, 4 parts of diboron trioxides and 1.5 parts of calcium oxide are uniformly mixed；
S2, grinding and sintering auxiliary agent: the mixture that S1 is obtained is added in nanon ball-mill, and dry ball milling to average grain diameter is 1 micron of powder；
S3, raw material mixing, compression moulding: powder obtained in S2 is uniformly mixed with 90 parts of boron carbide powders, uses pressure Machine compression moulding under the pressure of 25 MPa, wherein boron carbide powder was the boron carbide micro powder that partial size is micron after 800 meshes.
S4, low-temperature sintering: low-temperature sintering is carried out to the mixture that S3 is obtained in 550 DEG C of air atmospheres, obtains boron content For 63 ~ 71 wt%, density is 1.6 ~ 1.8 g/cm3, compression strength is the hydrogen-free neutron screen of high-intensitive high boron content of 29 ~ 65MPa Cover material.
NSM sample obtained in difference Example one and embodiment three uses WEW-300 type microcomputer to show universal test Machine carries out compressive property test to neutron shielding material.Wherein, the mass content of boron is about in the NSM sample that embodiment one obtains 63%, the mass content of boron is about 71% in the NSM sample that embodiment three obtains.
NSM sample in embodiment one and embodiment three is diameter 12mm, and the cylindric sample of height 40mm is put respectively On the sample stage of test machine, apply a stress, 0.3 KN/s of load rate records stress time curve.
Fig. 4 and Fig. 5 are referred to, as can be seen from Figure 4, the tensile strength of the NSM sample of embodiment one is 65.3 MPa, data Show the compression strength that the NSM sample of embodiment one is still done well.The tensile strength of NSM sample is 28.8 MPa in Fig. 5, Tensile strength decreases.It can be seen that NSM sample compression strength is about between 29 ~ 65MPa, and with boron content in NSM sample Increase, tensile strength decline.In general, the compressive property of the neutron shielding material obtained using preparation method of the invention Preferably.
Use above specific case is illustrated the present invention, is merely used to help understand the present invention, not to limit The system present invention.For those skilled in the art, according to the thought of the present invention, can also make several simple It deduces, deform or replaces.

Claims (8)

1. a kind of hydrogen-free neutron shielding material of high intensity high boron content, which is characterized in that the neutron shielding material includes following Component:
1 ~ 4 part of silica；
1 ~ 5 part of aluminum oxide；
3 ~ 8 parts of potassium phosphates；
1 ~ 4 part of diboron trioxide；
0.2 ~ 1.5 part of calcium oxide, and
80 ~ 90 parts of boron carbides；
Boron content in the neutron shielding material is 63 ~ 71 wt%.
2. the hydrogen-free neutron shielding material of high intensity high boron content according to claim 1, which is characterized in that the neutron screen The density for covering material is 1.6 ~ 1.8 g/cm3。
3. the hydrogen-free neutron shielding material of high intensity high boron content according to claim 1 or 2, which is characterized in that in described The compression strength of sub- shielding material is 29 ~ 65MPa.
4. a kind of method for preparing the hydrogen-free neutron shielding material of high-intensitive high boron content described in claim 1, which is characterized in that It will
1 ~ 4 part of silica；
1 ~ 5 part of aluminum oxide；
3 ~ 8 parts of potassium phosphates；
1 ~ 4 part of diboron trioxide；And
0.2 ~ 1.5 part of calcium oxide is ground to powder after being mixed, and is uniformly mixed with 80 ~ 90 parts of boron carbide powders, compression moulding, In 500 ~ 550 DEG C of air atmosphere low temperature sinterings, the neutron shielding material that boron content is 63 ~ 71 wt% is obtained.
5. the method for the hydrogen-free neutron shielding material of high intensity high boron content according to claim 4, which is characterized in that described Silica, aluminum oxide, potassium phosphate, diboron trioxide and calcium oxide are ground to the powder that average grain diameter is 1 ~ 5 micron.
6. the method for the hydrogen-free neutron shielding material of high intensity high boron content according to claim 4 or 5, which is characterized in that The boron carbide powder was the boron carbide micro powder that partial size is micron after 150 ~ 800 meshes.
7. the method for the hydrogen-free neutron shielding material of high intensity high boron content according to claim 4 or 5, which is characterized in that The pressure applied in the compression moulding is 10 ~ 25 MPa.
8. the method for the hydrogen-free neutron shielding material of high intensity high boron content according to claim 4 or 5, which is characterized in that The temperature of the air atmosphere low temperature sintering is 510 ~ 540 DEG C.
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