CN102280156A - Method for preparing aluminum-based boron carbide neutron absorption board - Google Patents

Method for preparing aluminum-based boron carbide neutron absorption board Download PDF

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CN102280156A
CN102280156A CN2011101698182A CN201110169818A CN102280156A CN 102280156 A CN102280156 A CN 102280156A CN 2011101698182 A CN2011101698182 A CN 2011101698182A CN 201110169818 A CN201110169818 A CN 201110169818A CN 102280156 A CN102280156 A CN 102280156A
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powder
boron carbide
plate
mould
neutron absorber
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CN102280156B (en
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吴岩
顾国兴
王保东
王文先
沈秋平
张鹏
黄然
奚梅英
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DALIAN BAOYUAN NUCLEAR EQUIPMENT CO LTD
SHANXI ZHONGTONG HIGH-TECH CO LTD
Shanghai Nuclear Engineering Research and Design Institute Co Ltd
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SHANXI ZHONGTONG HIGH-TECH CO LTD
Dalian Baoyuan Nuclear Equipment Co Ltd
Shanghai Nuclear Engineering Research and Design Institute Co Ltd
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Abstract

The invention relates to a method for preparing an aluminum-based boron carbide neutron absorption board. According to a requirement on nuclear device protection, the compact aluminum-based boron carbide neutron absorption board is formed by mixing aluminum powder, boron carbide powder, silicon powder, titanium powder and boracic acid crystal, performing powder metallurgy to make a rectangular board, and performing hot extrusion molding on the rectangular board on a pressing machine in a die in a heating state; the compound neutron absorption board is grey white; the neutron absorption rate is more than or equal to 90 percent, the boron carbide is distributed uniformly, and particles and a base body are tightly combined together; the micro hardness of the base body is up to 185.8HV and the micro hardness of the particles is up to 2,022.2HV; a corrosion resistance level on the surface of the board is -0.45 voltage, the anti-bending angle is more than or equal to 10 degrees, the tensile strength is more than or equal to 200 MPa, the fracture elongation rate is 1.8 percent and the fracture contractibility rate is more than or equal to 1.0 percent. The preparation method is advanced and rational in process, and is full and accurate in parameter; and the preparation method is an ideal method for preparing the aluminum-based boron carbide neutron absorption board.

Description

A kind of preparation method of aluminium base boron carbide neutron absorber plate
Technical field
The present invention relates to a kind of preparation method of aluminium base boron carbide neutron absorber plate, belong to the technical field of nonferrous metal powder metallurgy and plate forming, Enhancement Method.
Background technology
In nuclear device,, often adopt neutron material and technology to carry out shielding protection in order to prevent nuclear radiation.
The normal at present neutron absorbing material that adopts is lead-boron polythene, boracic polypropylene, and its advantage is that shielding construction is simple, and shield is in light weight, volume is little, but lead-boron polythene is easily aging, and the life-span is short, has limited its application; The cadmium plate also can be used as the neutron absorbing material, but cadmium is poisonous, and is carcinogenic; Boron steel also can be used as the neutron absorbing material, but the boron steel boron content is too low, is difficult to satisfy the shielding needs.
Boron carbide B 4C has higher neutron receptivity, its thermal-neutron capture cross-section height, capture spectra is wide, does not produce radioactive isotope, the Secondary radiation energy is low, and corrosion-resistant, Heat stability is good, the nuclear power station exterior wall of being everlasting pastes with the mosaic dress of boron carbide sintering, play intercept neutrons, but the boron carbide poor toughness, fragility is big, is difficult to make the neutron absorbing material of structure-function integration.
Metallic aluminium have preferably toughness, material light, easily extend, corrosion-resistant, plasticity is strong, does carrier with the metal aluminum or aluminum alloy, makes neutron absorber with boron carbide, make Metal Substrate neutron absorbing material, can improve toughness of material, can guarantee to have the neutron absorptive character again, but contain B 4The preparation of the Al based composites that C is higher and plate forming technology are also in inquiring into research.
Summary of the invention
Goal of the invention
The objective of the invention is situation at background technology, prepare the neutron absorbing material with aluminium powder, boron carbide powder, carry out powder metallurgy earlier, make blank, on hot press, in mould, be hot pressed into rectangle sheet material then, be aluminium base boron carbide neutron absorber plate material, so that as the neutron absorber plate of nuclear device, to increase substantially the ability of shielding neutron irradiation.
Technical scheme
The chemical substance material that the present invention uses is: aluminium powder, boron carbide powder, titanium valve, silica flour, boric acid crystal, graphite paper, fine sand, its value is as follows: be measurement unit with the gram
Figure BSA00000523016700021
The preparation method is as follows:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out quality purity control:
Figure BSA00000523016700022
(2) oxidation processes aluminium powder, boron carbide powder
1. aluminium powder is placed in the rustless steel container, place electric furnace then, be heated to 450 ℃ ± 5 ℃, carry out pre-oxidation, time 60min;
2. boron carbide powder is placed in the rustless steel container, place electric furnace then, carry out pre-oxidation, 400 ℃ ± 5 ℃ of oxidizing temperatures, time 90min;
(3) ball milling, sieve
With aluminium powder, boron carbide powder, titanium valve, silica flour, boric acid crystal respectively with the bowl mill ball milling, sieve, ball milling time 120min, sieve number 650 orders become fine powder behind the ball milling, fine powder particle diameter≤0.02mm;
(4) mixing fine powders
With aluminium powder, boron carbide powder, titanium valve, silica flour, boric acid crystal, in 65: 30: 2: 2: 1 ratio places batch mixer, mixes, and becomes mixing fine powders;
(5) powder metallurgy, base
1. the powder metallurgy base carries out in stainless steel mould, on the resistance heated state, pressing machine, and stainless steel mould is the open-close type cuboid, sticks on graphite paper earlier in the chamber, then mixing fine powders is added in the mould;
2. mould and mixing fine powders are placed on the pressing machine, pressurization 260T pre-molding, put into resistance-heated furnace then, be heated to 500 ℃ ± 5 ℃, constant temperature insulation 30min proceeds extruding with 260T pressure then, continues to be warming up to 600 ℃ ± 5 ℃, constant temperature, insulation 30min, and proceed to push with 260T pressure;
3. close resistance-heated furnace, make it naturally cool to 200 ℃ with stove;
4. open stainless steel mould, take out the powder metallurgy blank;
5. cool off in the fine sand, the powder metallurgy blank is imbedded in the fine sand, be cooled to 25 ℃, become the composite plate blank;
(6) be hot extruded into plate
1. the extruding of the rectangular billet behind the powder metallurgy is at the open-close type stainless steel mould, carry out on heated press;
2. mould is installed on the press base, place on the electric heater, lower bolster is vertically placed mold bottom, on lower bolster, evenly spread one deck graphite paper, then the composite plate blank behind the powder metallurgy is placed graphite paper top, evenly spread one deck graphite paper on composite plate blank top then, then cope match-plate pattern is pressed on the graphite paper, the pressure plare with pressing machine is pressed on the cope match-plate pattern then;
3. the electric resistance heater on the opening pressure machine base, 550 ℃~600 ℃ of heating-up temperatures;
4. the dynamo-electric machine of opening pressure pushes the composite plate blank, press pressure 260T, and composite plate is carried out plastic yield under pressure, and extends around in mould, becomes rectangular plate shape;
5. after composite plate blank and dies cavity size are coincide, stop pressurization, make it under heated condition, constant temperature leaves standstill 30min;
6. close electric resistance heater, make it naturally cool to 25 ℃;
7. rise pressing machine, open the mould open/close frame, take off template, composite plate, neutron absorbs the composite plate moulding;
8. with the cutting of neutron composite plate, finishing periphery, become: the aluminium base boron carbide neutron of 180 * 500 * 5mm absorbs composite board product;
(7) average tempering is handled
Neutron absorption composite plate to preparation places the tempering heat treatment stove to carry out average tempering processing, 450 ℃ ± 5 ℃ of temperatures, time 120min;
After the tempering, close tempering furnace, make it naturally cool to 25 ℃;
(8) detect, analyze, characterize
To pattern, color and luster, metallurgical structure, microhardness, the corrosion resistance of aluminium base boron carbide neutron absorber plate of preparation, neutron absorption rate detects, analyzes, characterizes;
Carry out the neutron absorption rate check and analysis with the neutron fluence rate instrument;
With electron microscope and scanning electron microscope composite plate transversal section, vertical section are carried out metallographic structure microstructure morphology analysis;
With the microhardness instrument composite plate is carried out the microhardness analysis;
Carry out bending resistance, tension analysis with universal testing machine;
Carry out the surface corrosion performance evaluation with the electrochemical corrosion test instrument;
Conclusion: Al base B 4The C neutron absorber plate is the canescence rectangular slab, neutron absorption rate 〉=90%; Boron carbide is evenly distributed, and particle combines with basal body interface closely, and the matrix microhardness is 185.8HV, the particle microhardness is 2022.2HV, and surperficial corrosion-resistant current potential is-0.45V that counter-bending angle is 〉=10 °, tensile strength 〉=200MPa, elongation after fracture 〉=1.8%, the shrinkage factor of having no progeny 〉=1.0%;
(9) store
Aluminium base boron carbide neutron absorber plate to preparation is packed with soft material, is stored in drying, clean environment, waterproof, protection against the tide, sun-proof, fire prevention, acid-proof alkali salt to corrode 20 ℃ ± 2 ℃ of storage temperatures, relative humidity≤10%.
Beneficial effect
The present invention compares with background technology has tangible advance; it is requirement at the nuclear device protection; prepare aluminium base boron carbide neutron absorber plate; adopt aluminium powder; boron carbide powder; titanium valve; silica flour; the boric acid crystal mixes; carry out powder metallurgy earlier and make the rectangular slab blank; then on pressing machine; under heated condition; carry out hot extrusion in mould, make the high aluminium base boron carbide neutron absorber plate of density, neutron absorber plate is a canescence; neutron absorption rate 〉=90%; boron carbide is evenly distributed, and particle and matrix bond are tight, and the matrix microhardness reaches 185.8HV; the particle microhardness reaches 2022.2HV; the corrosion-resistant current potential in surface is-0.45V that counter-bending angle is 〉=10 °, tensile strength 〉=200MPa; elongation after fracture 〉=1.8%, the shrinkage factor of having no progeny 〉=1.0%.
This preparation method's technology is rationally advanced, and parameter is accurately full and accurate, is the method for the very good aluminium base boron carbide neutron absorber plate of preparation.
Description of drawings
Fig. 1 is the constitutional diagram of aluminium base boron carbide neutron absorber plate powder metallurgy
Fig. 2 is the hot-forming constitutional diagram of aluminium base boron carbide neutron absorber plate
Fig. 3 is aluminium base boron carbide neutron absorber plate square section metallurgical structure figure
Fig. 4 is aluminium base boron carbide neutron absorber plate microstructure sem photograph
Shown in the figure, list of numerals is as follows:
1. press base, 2. well heater, 3. metallurgical powder mould, 4. movable rack, 5. cope match-plate pattern, 6. lower bolster, 7 graphite papers, 8. graphite paper, 9. metallurgical powder, 10. top board, 11. press rods, 12. pressure motors, 13. adjust handle, 14. backing plate, 15. neutron absorber plate moulds, 16. cope match-plate patterns, 17. lower bolster, 18. movable racks, 19. neutron composite plate blanks.
Embodiment:
The present invention will be further described below in conjunction with accompanying drawing:
Shown in Figure 1, be the constitutional diagram of aluminium base boron carbide neutron absorber plate powder metallurgy, the value of the powdered metallurgical material that preparation is used is to determine by the scope that sets in advance, and is measurement unit with the gram.
Preparation is on pressing machine, finishes in the open-close type stainless steel mould, and each position, annexation want correct, according to quantity proportioning, operation according to the order of sequence.
On press base 1 top is well heater 2, on well heater 2 tops is backing plate 14, put metallurgical powder mould 3 on backing plate 14 tops, mould 3 carries out the folding assembling by movable rack 4, metallurgical powder mould 3 inner bottom parts are lower bolster 6, lay one deck graphite paper 8 on lower bolster 6 tops, evenly put metallurgical powder 9 on graphite paper 8 tops, put graphite paper 7 on metallurgical powder 9 tops, put cope match-plate pattern 5 on graphite paper 7 tops, on cope match-plate pattern 5 tops by top board 10 glands of pressing machine, top board 10 tops connect press rods 11, press rods 11 tops connect pressure motor 12, promptly be provided with adjustment handle 13 on press rods 10 right sides, the heating-up temperature of well heater 2 adjustable metallurgical powders 9 is adjusted handle 13 and is adjusted mould and each position of pressing machine, the pressure of pressure motor 12 is exerted pressure to metallurgical powder 9 on demand, 9 one-tenth rectangle neutron absorber plates of metallurgical powder blank after heating is exerted pressure.
Powder metallurgy die is made of stainless steel material, is beneficial to the demoulding.
Shown in Figure 2, be the hot-forming constitutional diagram of aluminium base boron carbide neutron absorber plate, hot-forming on the pressing machine, carry out in the open-close type mould, it is correct that each position annexation is wanted, according to the order of sequence operation.
On press base 1 top is well heater 2, on well heater 2 tops is backing plate 14, place neutron absorber plate mould 15 on backing plate 14 tops, neutron absorber plate mould 15 is an open-close type, carry out the folding assembling by movable rack 18, neutron absorber plate mould 15 inner bottom parts are lower bolster 17, graphite paper 8 is placed on lower bolster 17 tops, neutron absorber plate blank 19 is placed on graphite paper 8 tops, put graphite paper 7 on neutron absorber plate blank 19 tops, put cope match-plate pattern 16 on graphite paper 7 tops, cope match-plate pattern 16 tops are top board 10, top board 10 tops connect press rods 11, press rods 11 tops connect pressure motor 12, promptly be provided with adjustment handle 13 on press rods 11 right sides, the heating-up temperature of well heater 2 adjustable neutron absorber plate blanks 19, adjust handle 13 and adjust top board 10 on demand, the position of press rods 11, pressing machine 12 is exerted pressure to neutron absorber plate blank 19 on demand, in heating, in the spinning process, neutron absorber plate blank 19 carries out plastic yield, become neutron absorber plate sheet material, i.e. neutron absorber plate.
The neutron absorber plate mould is made of the chrome-molybdenum steel of tool steel class, with high temperature resistant, intensity and the hardness that strengthens mould.
Shown in Figure 3, be neutron absorber plate square section metallurgical structure figure, among the figure as seen: adularescent, black particle in aluminum substrate, white particle are silicon or titanium, and black particle is a boron carbide, and boron carbide particles is evenly distributed in aluminum substrate, do not have obvious pore, defective.
Shown in Figure 4, be neutron absorber plate section microstructure sem photograph, among the figure as seen: adularescent, black particle in complex, white particle is silicon or titanium, black particle is a boron carbide, and the grey matrix is aluminium base, and boron carbide is evenly distributed in aluminium base, there is canescence interfacial reaction product on the boron carbide particles surface, at base aluminum, Ti and B 4Have interfacial reaction between C, reaction equation is as follows: B 4C+3Ti-2TiB 2+ TiC, the interfacial reaction product makes Al and B 4Wetting state between C is well improved.

Claims (3)

1. the preparation method of an aluminium base boron carbide neutron absorber plate is characterized in that: the chemical substance material that the present invention uses is: Al alloy powder, and boron carbide powder, titanium valve, silica flour, boric acid crystal, graphite paper, fine sand, its value is as follows: be measurement unit with the gram
Figure FSA00000523016600011
The preparation method is as follows:
(1) selected chemical substance material
To carry out selectedly to preparing required chemical substance material, and carry out quality purity control:
(2) oxidation processes aluminium powder, boron carbide powder
1. aluminium powder is placed in the rustless steel container, place electric furnace then, be heated to 450 ℃ ± 5 ℃, carry out pre-oxidation, time 60min;
2. boron carbide powder is placed in the rustless steel container, place electric furnace then, carry out pre-oxidation, 400 ℃ ± 5 ℃ of oxidizing temperatures, time 90min;
(3) ball milling, sieve
With aluminium powder, boron carbide powder, titanium valve, silica flour, boric acid crystal respectively with the bowl mill ball milling, sieve, ball milling time 120min, sieve number 650 orders become fine powder behind the ball milling, fine powder particle diameter≤0.02mm;
(4) mixing fine powders
With aluminium powder, boron carbide powder, titanium valve, silica flour, boric acid crystal fine powder, in 65: 30: 2: ratio placed batch mixer in 2: 1, and the mixing that stirs becomes mixing fine powders;
(5) powder metallurgy, base
1. powder metallurgy, base carry out on the resistance heated pressing machine in stainless steel mould, and stainless steel mould is the open-close type cuboid, stick on graphite paper earlier in the chamber, then mixing fine powders are added in the mould;
2. mould and mixing fine powders are placed on the pressing machine, pressurization 260T pre-molding is put into resistance-heated furnace then, is heated to 500 ℃ ± 5 ℃.Constant temperature insulation 30min pushes with 260T then, continues to be warming up to 600 ℃ ± 5 ℃, constant temperature, insulation 30min, and proceed to push with 260T pressure;
3. close resistance-heated furnace, make it naturally cool to 200 ℃ with stove;
4. open stainless steel mould, take out the powder metallurgy blank;
5. cool off in the fine sand, the powder metallurgy blank is imbedded in the fine sand, be cooled to 25 ℃, become the composite plate blank;
(6) be hot extruded into plate
1. the extruding of the rectangular billet behind the powder metallurgy is at the open-close type stainless steel mould, carry out on heated press;
2. mould is installed on the press base, place on the electric heater, lower bolster is vertically placed mold bottom, on lower bolster, evenly spread one deck graphite paper, then the composite plate blank behind the powder metallurgy is placed dag top, evenly spread one deck graphite paper on composite plate top then, then cope match-plate pattern is pressed on the graphite paper, the pressure plare with pressing machine is pressed on the cope match-plate pattern then;
3. the electric resistance heater on the opening pressure machine base, 550 ℃-600 ℃ of heating-up temperatures;
4. the dynamo-electric machine of opening pressure pushes the composite plate blank, press pressure 260T, and composite plate is carried out plastic yield under pressure, and extends around in mould, becomes rectangular plate shape;
5. after composite plate blank and dies cavity size are coincide, stop pressurization, make it under heated condition, constant temperature leaves standstill 30min;
6. close electric resistance heater, make it naturally cool to 25 ℃;
7. rise pressing machine, open the mould open/close frame, take off template, composite plate, neutron absorbs the composite plate moulding;
8. with the cutting of neutron composite plate, finishing periphery, become: the aluminium base boron carbide neutron of 180 * 500 * 5mm absorbs composite board product;
(7) average tempering is handled
Neutron absorption composite plate to preparation places the tempering heat treatment stove to carry out average tempering processing, 450 ℃ ± 5 ℃ of temperatures, time 120min;
After the tempering, close tempering furnace, make it naturally cool to 25 ℃;
(8) detect, analyze, characterize
To pattern, color and luster, metallurgical structure, microhardness, the corrosion resistance of aluminium base boron carbide neutron absorber plate of preparation, neutron absorption rate detects, analyzes, characterizes:
Carry out the neutron absorption rate check and analysis with the neutron fluence rate instrument;
With electron microscope and scanning electron microscope composite plate transversal section, vertical section are carried out metallographic structure microstructure morphology analysis;
With the microhardness instrument composite plate is carried out the microhardness analysis;
Carry out the surface corrosion performance evaluation with the electrochemical corrosion test instrument;
Carry out bending resistance, tension analysis with universal testing machine;
Conclusion: Al base B 4The C neutron absorber plate is the canescence rectangular slab, neutron absorption rate 〉=90%; Boron carbide is evenly distributed, and particle combines with basal body interface closely, and the matrix microhardness is 185.8HV, the particle microhardness is 2022.2HV, and surperficial corrosion-resistant current potential is-0.45V that counter-bending angle is 〉=10 °, tensile strength 〉=200MPa, elongation after fracture 〉=1.8%, the shrinkage factor of having no progeny 〉=1.0%.
(9) store
Aluminium base boron carbide neutron absorber plate to preparation is packed with soft material, is stored in drying, clean environment, waterproof, protection against the tide, sun-proof, fire prevention, acid-proof alkali salt to corrode 20 ℃ ± 2 ℃ of storage temperatures.Relative humidity≤10%.
2. the preparation method of a kind of aluminium base boron carbide neutron absorber plate according to claim 1, its feature in: on press base (1) top is well heater (2), on well heater (2) top is backing plate (14), put metallurgical powder mould (3) on backing plate (14) top, mould (3) carries out the folding assembling by movable rack (4), metallurgical powder mould (3) inner bottom part is lower bolster (6), lay one deck graphite paper (8) on lower bolster (6) top, evenly put metallurgical powder (9) on graphite paper (8) top, put graphite paper (7) on metallurgical powder (9) top, put cope match-plate pattern (5) on graphite paper (7) top, on cope match-plate pattern (5) top by top board (10) gland of pressing machine, top board (10) top connects press rods (11), press rods (11) top connects pressure motor (12), promptly be provided with adjustment handle (13) on press rods (10) right side, the heating-up temperature of the adjustable metallurgical powder of well heater (2) (9), adjust handle (13) and adjust mould and each position of pressing machine, the pressure of pressure motor (12) is exerted pressure to metallurgical powder (9) on demand, and metallurgical powder (9) became rectangle neutron absorber plate blank after heating was exerted pressure.
3. the preparation method of a kind of aluminium base boron carbide neutron absorber plate according to claim 1, it is characterized in that: on press base (1) top is well heater (2), on well heater (2) top is backing plate (14), place neutron absorber plate mould (15) on backing plate (14) top, neutron absorber plate mould (15) is an open-close type, carry out the folding assembling by movable rack (18), neutron absorber plate mould (15) inner bottom part is lower bolster (17), graphite paper (8) is placed on lower bolster (17) top, neutron absorber plate blank (19) is placed on graphite paper (8) top, put graphite paper (7) on neutron absorber plate blank (19) top, put cope match-plate pattern (16) on graphite paper (7) top, cope match-plate pattern (16) top is top board (10), top board (10) top connects press rods (11), press rods (11) top connects pressure motor (12), promptly be provided with adjustment handle (13) on press rods (11) right side, the heating-up temperature of well heater (2) is adjustable neutron absorber plate blank (19), adjust handle (13) and adjust top board (10) on demand, the position of press rods (11), pressing machine (12) is exerted pressure to neutron absorber plate blank (19) on demand, in heating, in the spinning process, neutron absorber plate blank (19) carries out plastic yield, become neutron absorber plate sheet material, i.e. neutron absorber plate.
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