CN104190914B - Method for preparing boron, lead and aluminum composite board preventing X rays, gamma rays and neutron irradiation - Google Patents

Method for preparing boron, lead and aluminum composite board preventing X rays, gamma rays and neutron irradiation Download PDF

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Publication number
CN104190914B
CN104190914B CN201410413729.1A CN201410413729A CN104190914B CN 104190914 B CN104190914 B CN 104190914B CN 201410413729 A CN201410413729 A CN 201410413729A CN 104190914 B CN104190914 B CN 104190914B
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boron
plumbous
aluminum composite
rolling
roll
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CN104190914A (en
Inventor
张鹏
王文先
陈洪胜
李宇力
张哲维
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Taiyuan University of Technology
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Taiyuan University of Technology
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Abstract

The invention relates to a method for preparing a boron, lead and aluminum composite board preventing X rays, gamma rays and neutron irradiation to overcome the defect that a nuclear radiation and ray shielding material is single in shielding property. According to the method, aluminum powder, boron carbide powder and lead powder serve as raw materials, ball grinding, powder processing, material mixing, microwave heating, vacuum hot pressing blank stamping, and heating rolling forming are carried out, and then the boron, lead and aluminum composite board is prepared. The preparing method is advanced in technology, data are accurate and detailed, the prepared boron, lead and aluminum composite board has a good ray and neutron irradiation shielding effect, the X-ray shielding rate is larger than or equal to 95 percent, the gamma-ray shielding rate is larger than or equal to 40 percent, the neutron absorptivity is larger than or equal to 90 percent, boron carbide is evenly distributed, particles and a base body are combined tightly, high mechanical strength is achieved, the surface microhardness reaches 186.3 HV, the bending angle is larger than or equal to 15 degrees, the tensile strength is 305 MPa, the elongation after fracture is larger than or equal to 6 percent, the mechanical property and the shielding property of the boron, lead and aluminum composite board are improved, and the boron, lead and aluminum composite board can be used for single irradiation protection and can also be used for various types of radiation protection.

Description

A kind of preparation method protecting the plumbous aluminum composite plate of boron of X, gamma-rays and neutron irradiation
Technical field
The present invention relates to a kind of preparation method protecting the plumbous aluminum composite plate of boron of X, gamma-rays and neutron irradiation, belong to the technical field of the preparations and applicatio of radiation protection and nuclear radiation protection material.
Background technology
Nuclear energy has become one of the most potential energy in the world today, nuclear fuel in nuclear power station and spentnuclear fuel can produce harmful X, gamma-rays and neutron irradiation in use, storage and transportation, therefore, shielding material is adopted harm ray to be shielded to the key issue becoming and must solve in nuclear energy uses process.
At present, the shielding material of nuclear fuel and spentnuclear fuel mainly contains lead-boron polythene, lead base boron carbide composite material, boron stainless steel material; Lead element has good shield effectiveness to X, gamma-rays, boron element has higher neutron absorption cross-section, although these materials have unique protective characteristic, be difficult to take into account the protection effect to multiple ray, its use under nuclear fuel and the complicated radiation condition of spentnuclear fuel is restricted.
Summary of the invention
Goal of the invention
The object of the invention is the deficiency for background technology, adopt vacuum hot-pressing, by surface alloying process, batch mixing base, cold pressing, sinter, hot rolling, make boron lead aluminum composite plate, make it not only can protect X, gamma-rays, but also maskable neutron irradiation, comprehensively to improve protection effect.
Technical scheme
The chemical substance material that the present invention uses is: aluminium powder, boron carbide powder, lead powder, absolute ethyl alcohol, graphite cake, graphite paper, sand paper, and it is as follows that it prepares consumption: with gram, milliliter, millimeter for measurement unit
Preparation method is as follows:
(1) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity control:
(2) mixing and ball milling, powder process
Take aluminium powder 1000g ± 0.01g, lead powder 600g ± 0.01g, boron carbide powder 400g ± 0.01g, be placed in ball mill, carry out mixing and ball milling, ball milling speed 200r/min, then sieves with 600 eye mesh screens, ball milling, sieves and repeatedly carries out, become mixing fine powders, fine particle diameter≤0.023mm;
(3) the plumbous aluminium base of boron is prepared in heating using microwave, vacuum hotpressing
The preparation of the plumbous aluminium base of boron is carried out on vacuum hot pressing formation machine, completes in heating using microwave, vacuum state, course of exerting pressure;
1. open-close type graphite jig is prepared
By graphite cake machine cuts, be assembled into rectangle retractable die, mold cavity is of a size of 80mm × 90mm × 90mm, and mold cavity surface roughness is Ra 0.08-0.016 μm;
2. feed
Open-close type graphite jig is vertically placed in the autoclave of vacuum hot pressing formation machine;
Bottom graphite block pad to mold cavity, graphite paper dress is attached to bottom open-close type graphite jig and on inwall;
The mixing fine powders of the aluminium powder prepared by ball milling, lead powder, boron carbide powder evenly loads in mold cavity;
At mixing fine powders top placing graphite paper;
On graphite paper top, graphite block is pushed down;
Graphite block top is fastened by upper holder block, and upper holder block top connects the pressure motor on footstock top;
3. open vavuum pump, extract air in autoclave, make vacuum in still reach 0.1Pa;
4. the microwave applicator in autoclave is opened, heated graphite mould and interior mixing fine powders thereof, heating-up temperature 600 DEG C ± 2 DEG C;
In microwave heating process, open the pressure motor on vacuum hot pressing formation machine, the mixing fine powders in graphite jig is exerted pressure, pressure of exerting pressure 100MPa;
Heat the time 90min that exerts pressure;
In heating, course of exerting pressure, the mixing fine powders in graphite jig is shaped to blank;
5. close microwave applicator, stop heating, make blank under vacuum conditions, under pressure of exerting pressure, be cooled to 25 DEG C;
6. close vavuum pump, make pressure in still return to 1 atmospheric pressure; Closedown is exerted pressure motor, stops exerting pressure to the blank in graphite jig;
7. drive still, take out open-close type graphite jig;
8. die sinking, opens graphite jig movable rack, takes out blank, i.e. the plumbous aluminium base of boron;
(4) the plumbous aluminum composite plate of hot-roll forming boron
The hot-roll forming of the plumbous aluminum composite plate of boron carries out on roller mill, completes under heating, three passage rolling states;
1. annealing in process, is placed in annealing furnace by plumbous for boron aluminium base, carries out homo genizing annelaing process, annealing temperature 580 DEG C, annealing time 12h;
2. the upper and lower roll heater on roller mill is opened, heating-up temperature 450 DEG C, and constant;
3. the first passage amount of rolling adjustment top and bottom rolls spacing of the plumbous aluminium base of boron is pressed;
4. open the rotating mechanism of top and bottom rolls, the rotation direction of topping roll is counterclockwise, and the rotation direction of bottom roll is that top and bottom rolls velocity of rotation is 10r/min clockwise, and the rolling direction of the plumbous aluminium base of boron is rolling from left to right;
5. be placed in from left to right between top and bottom rolls by plumbous for the boron of annealing in process aluminium base, carry out the first passes, rolling thickness deflection is 20%;
6. press boron plumbous aluminium base second pass deformation adjustment top and bottom rolls spacing, be placed in from left to right between top and bottom rolls by plumbous for the boron of annealing in process aluminium base, carry out the second passes, rolling thickness deflection is 15%;
7. press boron plumbous aluminium base the 3rd pass deformation adjustment top and bottom rolls spacing, be placed in from left to right between top and bottom rolls by plumbous for the boron of annealing in process aluminium base, carry out the 3rd passes, rolling thickness deflection is 15%;
After overall rolling, become the plumbous aluminum composite plate of boron;
(5) lonneal
Plumbous for boron after rolling aluminum composite plate is placed in heat-treatment furnace and carries out lonneal, temperature 180 DEG C, tempering time 8h;
(6) clear up, clean
Plumbous for boron after tempering aluminum composite plate is placed on steel flat board, by sand papering periphery and upper and lower surface, makes any surface finish;
(7) clean
Boron after cleaning is clean plumbous aluminum composite plate washes of absolute alcohol periphery and upper and lower surface, make clean surface;
(8) analysis and characterization is detected
The pattern of the plumbous aluminum composite plate of the boron of preparation, color and luster, Chemical Physics performance, mechanical property are detected, analyze, characterized;
Density and density contrast test is carried out with drainage;
Carry out neutron absorption rate with Am-Be neutron source and neutron fluence rate instrument and detect analysis;
Detect by the shielding properties of EG300F type x-ray system to the X-ray of 100KeV;
With radioactive source 60Co (1.33MeV), gamma-ray shielding properties is detected;
Hardness distribution tests is carried out with the digital microhardness instrument of HXD-1000TM;
Bending resistance, Analysis On Tensile is carried out with INSTRON-5544 electronic universal material testing machine;
Conclusion: the plumbous aluminum composite plate of boron is light grey sheet material, and panel density is 3.397g/cm 3, X-ray shielding rate>=95%, gamma ray shielding rate>=40%, neutron absorption rate>=90%, tensile strength is 305MPa, counter-bending angle>=15 °, elongation after fracture>=6%, and surface microhardness is 186.3HV.
Beneficial effect
The present invention has obvious advance compared with background technology, for nuclear radiation and the single drawback of ray protection material shielding properties, with boron carbide powder, aluminium powder, lead powder for raw material, by ball milling powder process batch mixing, heating using microwave, vacuum hotpressing base, hot-roll forming, make the plumbous aluminum composite plate of boron, this preparation technology is advanced, and data are accurately full and accurate, the plumbous aluminum composite plate of the boron made is light grey sheet material, and panel density is 3.397g/cm 3, X-ray shielding rate>=95%, gamma ray shielding rate>=40%, neutron absorption rate>=90%, tensile strength is 305MPa, counter-bending angle>=15 °, elongation after fracture>=6%, surface microhardness is 186.3HV, both can be used for tailored radiation protection, and can be used for again the protection to multiple radiation.
Accompanying drawing explanation
Fig. 1 boron plumbous aluminium base preparing processes figure
The state diagram of Fig. 2 boron plumbous aluminum composite plate hot-roll forming
The plumbous aluminum composite plate cross section metallurgical structure figure of Fig. 3 boron
Shown in figure, list of numerals is as follows:
1. vacuum hot pressing formation machine, 2. forming machine console, 3. footstock, 4. machine chamber, 5. workbench, 6. open-close type graphite jig, 7. the first graphite block, 8. the second graphite block, 9. the first graphite paper, 10. the second graphite paper, the plumbous aluminium base of 11. boron, 12. upper holder blocks, 13. pressure motors, 14. movable racks, 15. vavuum pumps, 16. vacuum valves, 17. vacuum tubes, 18. display screens, 19. indicator lamps, 20. power switches, 21. controller for vacuum pumps, 22. heating using microwave controllers, 23. heat time controllers, 24. microwave generators, 25. outer water circulation cooling tubes, 26. outer water circulation water intaking valves, 27. outer water circulation outlet valves, the plumbous aluminum composite plate of 30. boron, 31. roller mill bases, 32. roller mill footstocks, 33. left columns, 34. right columns, 35. topping roll rotating mechanisms, 36. topping roll resistance heaters, 37. topping rolls, 38. bottom rolls, 39. bottom roll resistance heaters, 40. bottom roll rotating mechanisms, 41. roller mill display screens, 42. roller mill indicator lamps, 43. roller mill power switches, 44. topping roll pivoting controllers, 45. bottom roll pivoting controllers, 46. topping roll heating controllers, 47. bottom roll heating controllers.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be boron plumbous aluminium base preparing processes figure, each position, annexation want correct, and proportioning according to quantity, operates according to the order of sequence.
The value of the chemical substance that preparation uses determines by the scope pre-set, with gram, milliliter, millimeter for measurement unit.
The preparation of the plumbous aluminium base of boron is carried out on vacuum hot pressing formation machine, completes in heating using microwave, vacuum state, course of exerting pressure;
Vacuum hot pressing formation machine is vertical, be forming machine console 2 in the bottom of vacuum hot pressing formation machine 1, top be footstock 3, inner be machine chamber 4; Be workbench 5 at machine chamber 4 inner bottom part, vertically open-close type graphite jig 6 on workbench 5, and fixed by movable rack 14; Be the first graphite block 7 at open-close type graphite jig 6 inner bottom part, be the first graphite paper 9 on the top of the first graphite block 7, the plumbous aluminium base 11 of boron is evenly put on the first graphite paper 9 top, be the second graphite paper 10 on plumbous aluminium base 11 top of boron, pushed down by the second graphite block 8 on the second graphite paper 10 top, fastened by upper holder block 12 on the second graphite block 8 top, upper holder block 12 top connects the pressure motor 13 on footstock 3 top; The inwall of vacuum hot pressing formation machine 1 is provided with microwave generator 24; In the outside of vacuum hot pressing formation machine 1 by outer water circulation cooling tube 25 around, the right part of outer water circulation cooling tube 25 is provided with outer water circulation water intaking valve 26, left part is provided with outer water circulation outlet valve 27; Be provided with vavuum pump 15 at the right lower quadrant of vacuum hot pressing formation machine 1, vavuum pump 15 is communicated with machine chamber 4 by vacuum valve 16, vacuum tube 17; Forming machine console 2 is provided with display screen 18, indicator lamp 19, power switch 20, controller for vacuum pump 21, heating using microwave controller 22, heat time controller 23.
Shown in Fig. 2, be the state diagram of boron plumbous aluminum composite plate hot-roll forming, each position, connecting relation want correct, arrange according to quantity, operate according to the order of sequence.
The hot rolling of the plumbous aluminum composite plate of boron carries out on roller mill, completes under heating, rolling state;
Roller mill is vertical, and the bottom of roller mill is roller mill base 31, is provided with left column 33, right column 34 about roller mill base 31 upper part, is roller mill footstock 32 on left column 33, right column 34 top, composition overall structure; Rolling rotating mechanism 35 on roller mill footstock 32 bottom connects, topping roll rotating mechanism 35 bottom connects upper rolling resistance heater 36, and topping roll resistance heater 36 bottom connects topping roll 37; Be provided with bottom roll rotating mechanism 40 on roller mill base 31 top, connect bottom roll resistance heater 39 on bottom roll rotating mechanism 40 top, bottom roll resistance heater 39 top connects bottom roll 38; It is the plumbous aluminum composite plate 30 of boron between topping roll 37 and bottom roll 38; The rotation direction of topping roll 37 is for rotating counterclockwise, and the rotation direction of bottom roll 38 is for rotating clockwise, and the rolling direction of the plumbous aluminum composite plate 30 of boron is rolling from left to right; Roller mill base 31 is provided with roller mill display screen 41, roller mill indicator lamp 42, roller mill power switch 43, topping roll pivoting controller 44, bottom roll pivoting controller 45, topping roll heating controller 46, bottom roll heating controller 47.
Shown in Fig. 3, be boron plumbous aluminum composite plate cross section shape appearance figure, as shown in the figure, white base is 6061 alloy matrix aluminums, and the Metal Phase of grey uniform disperse in matrix is plumbous, and the particle be uniformly distributed in the base is B 4c particle, particle is soilless sticking phenomenon in the base.

Claims (2)

1. one kind is protected the preparation method of the plumbous aluminum composite plate of boron of X, gamma-rays and neutron irradiation, it is characterized in that: the chemical substance material of use is: aluminium powder, boron carbide powder, lead powder, absolute ethyl alcohol, graphite cake, graphite paper, sand paper, it is as follows that it prepares consumption: with gram, milliliter, millimeter for measurement unit
Preparation method is as follows:
(2) selected chemical substance material
To carry out selected to the chemical substance material that preparation uses, and carry out quality purity control:
(2) mixing and ball milling, powder process
Take aluminium powder 1000g ± 0.01g, lead powder 600g ± 0.01g, boron carbide powder 400g ± 0.01g, be placed in ball mill, carry out mixing and ball milling, ball milling speed 200r/min, then sieves with 600 eye mesh screens, ball milling, sieves and repeatedly carries out, become mixing fine powders, fine particle diameter≤0.023mm;
(3) the plumbous aluminium base of boron is prepared in heating using microwave, vacuum hotpressing
The preparation of the plumbous aluminium base of boron is carried out on vacuum hot pressing formation machine, completes in heating using microwave, vacuum state, course of exerting pressure;
1. open-close type graphite jig is prepared
By graphite cake machine cuts, be assembled into rectangle retractable die, mold cavity is of a size of 80mm × 90mm × 90mm, and mold cavity surface roughness is Ra 0.08-0.016 μm;
2. feed
Open-close type graphite jig is vertically placed in the autoclave of vacuum hot pressing formation machine;
Bottom graphite block pad to mold cavity, graphite paper dress is attached to bottom open-close type graphite jig and on inwall;
The mixing fine powders of the aluminium powder prepared by ball milling, lead powder, boron carbide powder evenly loads in mold cavity;
At mixing fine powders top placing graphite paper;
On graphite paper top, graphite block is pushed down;
Graphite block top is fastened by upper holder block, and upper holder block top connects the pressure motor on footstock top;
3. open vavuum pump, extract air in autoclave, make vacuum in still reach 0.1Pa;
4. the microwave applicator in autoclave is opened, heated graphite mould and interior mixing fine powders thereof, heating-up temperature 600 DEG C ± 2 DEG C;
In microwave heating process, open the pressure motor on vacuum hot pressing formation machine, the mixing fine powders in graphite jig is exerted pressure, pressure of exerting pressure 100MPa;
Heat the time 90min that exerts pressure;
In heating, course of exerting pressure, the mixing fine powders in graphite jig is shaped to blank;
5. close microwave applicator, stop heating, make blank under vacuum conditions, under pressure of exerting pressure, be cooled to 25 DEG C;
6. close vavuum pump, make pressure in still return to 1 atmospheric pressure; Closedown is exerted pressure motor, stops exerting pressure to the blank in graphite jig;
7. drive still, take out open-close type graphite jig;
8. die sinking, opens graphite jig movable rack, takes out blank, i.e. the plumbous aluminium base of boron;
(4) the plumbous aluminum composite plate of hot-roll forming boron
The hot-roll forming of the plumbous aluminum composite plate of boron carries out on roller mill, completes under heating, three passage rolling states;
1. annealing in process, is placed in annealing furnace by plumbous for boron aluminium base, carries out homo genizing annelaing process, annealing temperature 580 DEG C, annealing time 12h;
2. the upper and lower roll heater on roller mill is opened, heating-up temperature 450 DEG C, and constant;
3. the first passage amount of rolling adjustment top and bottom rolls spacing of the plumbous aluminium base of boron is pressed;
4. open the rotating mechanism of top and bottom rolls, the rotation direction of topping roll is counterclockwise, and the rotation direction of bottom roll is that top and bottom rolls velocity of rotation is 10r/min clockwise, and the rolling direction of the plumbous aluminium base of boron is rolling from left to right;
5. be placed in from left to right between top and bottom rolls by plumbous for the boron of annealing in process aluminium base, carry out the first passes, rolling thickness deflection is 20%;
6. press boron plumbous aluminium base second pass deformation adjustment top and bottom rolls spacing, be placed in from left to right between top and bottom rolls by plumbous for the boron of annealing in process aluminium base, carry out the second passes, rolling thickness deflection is 15%;
7. press boron plumbous aluminium base the 3rd pass deformation adjustment top and bottom rolls spacing, be placed in from left to right between top and bottom rolls by plumbous for the boron of annealing in process aluminium base, carry out the 3rd passes, rolling thickness deflection is 15%;
After overall rolling, become the plumbous aluminum composite plate of boron;
(5) lonneal
Plumbous for boron after rolling aluminum composite plate is placed in heat-treatment furnace and carries out lonneal, temperature 180 DEG C, tempering time 8h;
(6) clear up, clean
Plumbous for boron after tempering aluminum composite plate is placed on steel flat board, by sand papering periphery and upper and lower surface, makes any surface finish;
(7) clean
Boron after cleaning is clean plumbous aluminum composite plate washes of absolute alcohol periphery and upper and lower surface, make clean surface;
(8) analysis and characterization is detected
The pattern of the plumbous aluminum composite plate of the boron of preparation, color and luster, Chemical Physics performance, mechanical property are detected, analyze, characterized;
Density and density contrast test is carried out with drainage;
Carry out neutron absorption rate with Am-Be neutron source and neutron fluence rate instrument and detect analysis;
Detect by the shielding properties of EG300F type x-ray system to the X-ray of 100KeV;
With radioactive source 60Co (1.33MeV), gamma-ray shielding properties is detected;
Hardness distribution tests is carried out with the digital microhardness instrument of HXD-1000TM;
Bending resistance, Analysis On Tensile is carried out with INSTRON-5544 electronic universal material testing machine;
Conclusion: the plumbous aluminum composite plate of boron is light grey sheet material, and panel density is 3.397g/cm 3, X-ray shielding rate>=95%, gamma ray shielding rate>=40%, neutron absorption rate>=90%, tensile strength is 305MPa, counter-bending angle>=15 °, elongation after fracture>=6%, and surface microhardness is 186.3HV.
2. a kind of preparation method protecting the plumbous aluminum composite plate of boron of X, gamma-rays and neutron irradiation according to claim 1, is characterized in that: the hot rolling of the plumbous aluminum composite plate of boron carries out on roller mill, completes under heating, rolling state;
Roller mill is vertical, the bottom of roller mill is roller mill base (31), left column (33), right column (34) is provided with about roller mill base (31) upper part, be roller mill footstock (32) on left column (33), right column (34) top, composition overall structure; Upper rolling rotating mechanism (35) is connected in roller mill footstock (32) bottom, topping roll rotating mechanism (35) bottom connects upper rolling resistance heater (36), and topping roll resistance heater (36) bottom connects topping roll (37); Bottom roll rotating mechanism (40) is provided with on roller mill base (31) top, connect bottom roll resistance heater (39) on bottom roll rotating mechanism (40) top, bottom roll resistance heater (39) top connects bottom roll (38); It is the plumbous aluminum composite plate (30) of boron between topping roll (37) and bottom roll (38); The rotation direction of topping roll (37) is for rotating counterclockwise, and the rotation direction of bottom roll (38) is for rotating clockwise, and the rolling direction of the plumbous aluminum composite plate (30) of boron is rolling from left to right; Roller mill base (31) is provided with roller mill display screen (41), roller mill indicator lamp (42), roller mill power switch (43), topping roll pivoting controller (44), bottom roll pivoting controller (45), topping roll heating controller (46), bottom roll heating controller (47).
CN201410413729.1A 2014-08-21 2014-08-21 Method for preparing boron, lead and aluminum composite board preventing X rays, gamma rays and neutron irradiation Expired - Fee Related CN104190914B (en)

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