CN104498754A - Preparation method of magnesium alloy-based neutron shielding composite material - Google Patents
Preparation method of magnesium alloy-based neutron shielding composite material Download PDFInfo
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- CN104498754A CN104498754A CN201410791007.XA CN201410791007A CN104498754A CN 104498754 A CN104498754 A CN 104498754A CN 201410791007 A CN201410791007 A CN 201410791007A CN 104498754 A CN104498754 A CN 104498754A
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- magnesium alloy
- matrix material
- neutron shield
- alloy base
- pressed sintering
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000002131 composite material Substances 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 28
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 21
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 18
- 229910052796 boron Inorganic materials 0.000 claims abstract description 13
- 238000001125 extrusion Methods 0.000 claims abstract description 11
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000002585 base Substances 0.000 claims description 65
- 239000011159 matrix material Substances 0.000 claims description 58
- 238000005245 sintering Methods 0.000 claims description 46
- 239000000843 powder Substances 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 229910002804 graphite Inorganic materials 0.000 claims description 24
- 239000010439 graphite Substances 0.000 claims description 24
- 239000000498 cooling water Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 7
- 238000004826 seaming Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000007872 degassing Methods 0.000 claims description 6
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000007669 thermal treatment Methods 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- 239000010959 steel Substances 0.000 claims description 4
- 238000005054 agglomeration Methods 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 2
- 239000000284 extract Substances 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 239000004576 sand Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- 239000007779 soft material Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000005684 electric field Effects 0.000 abstract description 2
- 238000007731 hot pressing Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract description 2
- 238000007599 discharging Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 238000012986 modification Methods 0.000 abstract 1
- 238000012876 topography Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000001192 hot extrusion Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000005275 alloying Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- YZDZYSPAJSPJQJ-UHFFFAOYSA-N samarium(3+);trinitrate Chemical compound [Sm+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YZDZYSPAJSPJQJ-UHFFFAOYSA-N 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000005251 gamma ray Effects 0.000 description 1
- 229910001234 light alloy Inorganic materials 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
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- Powder Metallurgy (AREA)
- Particle Accelerators (AREA)
Abstract
The invention relates to a preparation method of a magnesium alloy-based neutron shielding composite material. Aiming at an actual condition of nuclear radiation protection, rare-earth elements samarium and boron are good in neutron absorptivity; the rare-earth element samarium can have a modification effect on magnesium alloy; a plasma discharging and hot pressing technology is adopted to prepare a magnesium alloy-based neutron shielding composite material blank in the presence of an electric field at pressurization and vacuum conditions; a plasma-discharged and hot-pressed blank is beneficial for interface bonding; particles between components are uniformly distributed; the heating speed is high; oxidation pollution of the material can be effectively prevented under a vacuum environment; the blank is subjected to thermal extrusion molding, so the distribution uniformity of the particles is further improved; the mechanical properties of the material are improved; the preparation method is advanced in process and precise and accurate in data; the neutron absorptivity of the magnesium alloy-based neutron shielding composite material is as high as 97%; the density of the material is as high as 99%; the hardness of the material is as high as 140HV; the magnesium alloy-based neutron shielding composite material is a composite material which is light, high in strength and good in neutron shielding properties.
Description
Technical field
The present invention relates to a kind of preparation method of magnesium alloy base neutron shield matrix material, belong to the technical field of non-ferrous metal alloy preparations and applicatio.
Background technology
Magnesium alloy is that a kind of high-strength light alloy, electrical and thermal conductivity performance are good, and have good capability of electromagnetic shielding, wide model is applied to aerospace, automobile making and electronics industry; Magnesium alloy because neutron-absorption cross-section is little, Nai Gaore, resistance to surface heat flow and resistance to strong gamma-ray irradiation, can CO be kept out within 500 DEG C
2corrosion, in nuclear industry field, obtain good application.
In order to improve the structure properties of magnesium alloy, often add rare earth element in the magnesium alloy, to improve the mechanical property of magnesium alloy, adding of rare earth element can purify melt, refined crystalline strengthening, solution strengthening, dispersion-strengthened, improve the corrosion resistance nature of magnesium alloy, rare earth element is again good neutron absorber, and neutron-absorption cross-section is large, is good neutron shield constituent element; But rare earth element add-on is in the magnesium alloy restricted, add-on is too much, can affect the use properties of magnesium alloy; Boron is good neutron-absorbing material, and neutron-absorption cross-section is large, and boron is combined with magnesium alloy, and be effective neutron shielding material, boron has the character that density is low, intensity is high and fusing point is high; In order to obtain efficient neutron shield performance and good mechanical property, in magnesium alloy substrate, adding samarium and boron, neutron shield matrix material can be prepared.
Adopt plasma discharge hot pressed sintering base, magnesium alloy base neutron shield matrix material is prepared in pressing machine extruding, samarium and boron can be made to be evenly distributed in the middle of magnesium alloy substrate, the interface cohesion between constituent element is conducive under the effect of plasma discharge hot pressed sintering, plasma discharge hot pressed sintering heat-up rate is fast, it is short to prepare the blank time, growing up of matrix grain can be suppressed, blank is after extruding, samarium can be improved, the distributing homogeneity of boron in magnesium alloy substrate, improve the density of material, squeeze out difform section bar, it is a kind of practicable material preparation method.
Summary of the invention
Goal of the invention
The object of the invention is the situation for background technology, with magnesium alloy powder, boron powder, samarium powder for raw material, employing plasma discharge hot pressed sintering prepares blank, pressing machine is crushed to magnesium alloy base neutron shield matrix material, to improve the density of neutron shield matrix material, corrosion-resistant and mechanical property, to improve nuclear defence performance.
Technical scheme
The chemical substance material that the present invention uses is: magnesium alloy powder, boron powder, samarium powder, dehydrated alcohol, graphite paper, sand paper, and it is as follows that its combination prepares consumption: with gram, milliliter, millimeter for measure unit
Preparation method is as follows:
(1) cylindrical mold is prepared
Cylindrical mold graphite material makes, and mold cavity is of a size of Φ 40mm × 80mm, and mold cavity surfaceness is Ra 0.08-0.16 μm;
(2) dehumidifying, degassing processing magnesium alloy powder
Magnesium alloy powder is placed in quartz container, is then placed in vacuum furnace dry, drying temperature 50 DEG C, vacuum tightness≤2Pa, time of drying 30min;
(3) dehumidifying, degassing processing samarium powder
Samarium powder is placed in quartz container, is then placed in vacuum furnace dry, drying temperature 50 DEG C, vacuum tightness≤2Pa, time of drying 20min;
(4) dehumidifying, degassing processing boron powder
Boron powder is placed in quartz container, is then placed in vacuum furnace dry, drying temperature 100 DEG C, vacuum tightness≤2Pa, time of drying 20min;
(5) prepare burden
Batching is carried out in vacuum glove box, and vacuum glove box case pressure is-0.1mbar, water-content < 0.1ppm, oxygen level < 0.1ppm;
Take magnesium alloy powder 170g ± 0.01g, boron powder 20g ± 0.01g, samarium powder 10g ± 0.01g, be placed in ball grinder, ball sealer grinding jar;
Magnesium alloy powder: boron powder: samarium powder=17:2:1;
(6) ball mill mixing
The ball grinder of powder mix will be housed as on ball mill, ball milling mixes powder time 2h, drum's speed of rotation 1200rpm, and ball milling becomes mixing fine powders;
(7) feed
Ball grinder is placed in vacuum glove box, mixing fine powders is added in circular graphitic mould;
In mold cavity, place mould lower cushion block, at mould lower cushion block top placing graphite paper, place mixing fine powders on graphite paper top, at mixing fine powders top placing graphite paper, place mould seaming chuck on graphite paper top;
(8) hot pressed sintering of magnesium alloy base neutron shield matrix material blank
The hot pressed sintering of magnesium alloy base neutron shield matrix material carries out in plasma discharge hot-pressed sintering furnace, under vacuum conditions, heating, to complete in course of exerting pressure;
1. open plasma discharge hot-pressed sintering furnace, charged circular die is placed in lower electrode top, top electrode is pushed down cylindrical mold, and fixing;
Close plasma discharge hot-pressed sintering furnace;
2. open water device for cooling water pump, carries out outer water cycle cooling;
3. open vacuum pump, extract furnace air, make pressure≤2Pa in stove;
4. opening pressure motor, exerts pressure to mould, and exert pressure pressure 25kN;
5. open electric pulse heating device, Heating temperature, time were undertaken by four stages:
First stage: temperature is 20 DEG C ~ 350 DEG C, time 10min;
Subordinate phase: temperature is 350 DEG C ~ 450 DEG C, time 5min;
Phase III: temperature is 450 DEG C ~ 500 DEG C, time 5min;
Fourth stage: temperature is 500 DEG C of constant temperature insulations, time 10min;
6. after plasma discharge hot pressed sintering, close plasma discharge hot-pressed sintering furnace, stop heating, stop exerting pressure, cool to 25 DEG C with the furnace;
7. die sinking, opens plasma discharge hot-pressed sintering furnace, takes out graphite jig, opens graphite jig, takes out sintering block, is magnesium alloy base neutron shield matrix material blank;
(9) thermal treatment
The thermal treatment of magnesium alloy base neutron shield matrix material blank is carried out in resistance heading furnace, and cylinder blank is put into resistance heading furnace, and thermal treatment temp is 415 DEG C, and heat-up time is 24h;
Then 25 DEG C are cooled to the furnace;
(10) extruding of magnesium alloy base neutron shield matrix material
The extrusion molding of magnesium alloy base neutron shield matrix material is carried out on vertical hydraulic pressing machine, completes under heating, pressurization and Extruding die guide functions;
1. prepare extrusion mould, extrusion mould 4Cr5MoSiV1 hot-work die steel makes, and extrusion mould is made up of Extruding die, extruding punch and mould container;
2. extrusion mould cylindrical shell is placed on the worktable of vertical press, puts Extruding die in mould container inside, blank is placed in Extruding die, put extruding punch on blank top, resistance heater is set around mould container;
3. opening resistor well heater, heating mould and blank, Heating temperature is 350 DEG C ± 5 DEG C, constant temperature soaking time 60min;
4. open vertical press, extruding punch extrudes in Extruding die preformed body, and squeeze pressure is 100kN, is squeezed into rectangular plate, stops heating, make it naturally cool to 25 DEG C after extruding;
Die sinking after extruding, takes out rectangular plate, is magnesium alloy base neutron shield matrix material;
(11) polishing, sanding process
The magnesium alloy base neutron shield matrix material of preparation is placed on steel flat board, with sand papering periphery and surface, makes it clean;
(12) clean, with washes of absolute alcohol magnesium alloy base neutron shield composite material surface, make it clean;
(13) detect, analyze, characterize
The pattern of magnesium alloy base neutron shield matrix material of preparation, color and luster, chemical physics performance, mechanical property are detected, analyze, characterized;
The density test of material is carried out with Archimedes's drainage;
Hardness performance analysis is carried out with microhardness instrument;
Analysis on Microstructure is carried out with metaloscope instrument;
The test of shielding Neutron properties is carried out by Am-Be neutron source;
Conclusion: magnesium alloy base neutron shield matrix material is silvery white, and density reaches 99%, and samarium particle and boron particles agglomeration do not appear in material internal, samarium particle and boron particles are evenly distributed between magnesium alloy particles, between particle, interface cohesion is good, and hardness reaches 140HV, and neutron-absorbing performance reaches 97%;
(14) store
The magnesium alloy base neutron shield matrix material soft material of preparation is packed, is stored in cleaning, dry environment, moistureproof, sun-proof, anti-acid-alkali salt to corrode, storing temp 20 DEG C, relative humidity≤10%.
Beneficial effect
The present invention has obvious advance compared with background technology, the practical situation for nuclear radiation protection, Samarium Nitrate and boron have good neutron-absorbing performance, Samarium Nitrate can play modifying function to magnesium alloy, adopt plasma discharge hot pressing and sintering technique, magnesium alloy base neutron shield matrix material blank is prepared under electric field, pressurization and vacuum condition, plasma discharge hot pressed sintering blank is conducive to interface cohesion, even particle distribution between each constituent element, rate of heating is fast, effectively can prevent the oxidation stain of material under vacuum environment; Blank is through hot extrusion molding, improve particle distribution uniformity, improve the mechanical property of material, this preparation method's technique is advanced, data are accurately full and accurate, and the neutron-absorbing performance of magnesium alloy base neutron shield matrix material reaches 97%, and density of material reaches 99%, material hardness reaches 140HV, is a kind of lightweight, high-strength, the matrix material with good neutron shield performance.
Accompanying drawing explanation
Fig. 1, the state graph of magnesium alloy base neutron shield matrix material blank hot pressed sintering
Fig. 2, magnesium alloy base neutron shield matrix material hot extrusion state graph
Fig. 3, magnesium alloy base neutron shield matrix material square section displaing micro tissue topography figure
Fig. 4, magnesium alloy base neutron shield matrix material profile displaing micro tissue topography figure
Shown in figure, list of numerals is as follows:
1, plasma discharge hot-pressed sintering furnace, 2, pressure motor, 3, top electrode, 4, furnace chamber, 5, vacuum pump, 6, upper holder block, 7, valve tube, 8, seaming chuck, 9, outer water cycle cooling tube, 10, second graphite paper, 11, magnesium alloy base neutron shield matrix material mixing fine powders, 12, cylindrical mold, 13, first graphite paper, 14, lower margin, 15, lower cushion block, 16, cooling water tank, 17, lower electrode, 18, worktable, 19, first left socle, 20, first right support, 21, cooling-water pump, 22, water-cooled tube, 23, electric control box, 24, first display screen, 25, first pilot lamp, 26, power switch, 27, controller for vacuum pump, 28, cooling-water pump controller, 29, pressure electric machine controller, 30, heating temperature control, 31, heat-up time controller, 32, first wire, 33, hydraulic press, 34, footstock, 35, hydraulic ram, 36, extruding punch, 37, resistance heater, 38, container, 39, Extruding die, 40, discharge hole, 41, base, 42, second left socle, 43, forcing spindle, 44, traverser, 45, top briquetting, 46, magnesium alloy base neutron shield Composite Sintering blank, 47, second wire, 48, second right support, 49, electrical control cubicles, 50, second display screen, 51, second pilot lamp, 52, power-supply controller of electric, 53, hydrauliccontroller, 54, resistive heating controller, 55, hydraulic power unit, 56, oil inlet pipe, 58, oil outlet pipe, 58, first hydraulicefficiency pressure gauge, 59, second hydraulicefficiency pressure gauge.
Embodiment:
Below in conjunction with accompanying drawing, the present invention will be further described:
Shown in Fig. 1, be the state graph of magnesium alloy base neutron shield matrix material blank hot pressed sintering, 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 measure unit.
The hot pressed sintering of magnesium alloy base neutron shield matrix material blank carries out in plasma discharge hot-pressed sintering furnace, under vacuum conditions, heating, to complete in course of exerting pressure;
Plasma discharge hot-pressed sintering furnace is vertical, and the bottom of plasma discharge hot-pressed sintering furnace 1 is worktable 18, and worktable 18 bottom supports fixing by the first left socle 19, first right support 20, be outer water cycle cooling tube 9 in plasma discharge hot-pressed sintering furnace outside, be furnace chamber 4 in plasma discharge hot-pressed sintering furnace 1 inside, in furnace chamber 4, bottom is lower electrode 17, lower electrode 17 top is lower cushion block 15, lower cushion block 15 top is lower margin 14, lower margin 14 stretches in cylindrical mold 12, lower margin 14 top is the first graphite paper 13, it is magnesium alloy base neutron shield matrix material mixing fine powders 11 on the first graphite paper 13 top, be the second graphite paper 10 on magnesium alloy base neutron shield matrix material mixing fine powders 11 top, be seaming chuck 8 on the second graphite paper 10 top, be upper holder block 6 on seaming chuck 8 top, be top electrode 3 on upper holder block 6 top, at top electrode 3 top Bonding pressure motor 2, be electric control box 23 at the right part of plasma discharge hot-pressed sintering furnace 1, being worktable 18 in the bottom of plasma discharge hot-pressed sintering furnace 1, electric control box 23, is vacuum pump 5 at the lower left part of worktable 18, is communicated with furnace chamber 4 on vacuum pump 5 top by valve tube 7, be cooling water tank 16 at worktable 18 lower right section, cooling water tank 16 top is provided with cooling-water pump 21, and cooling-water pump 21 is communicated with outer water cycle cooling tube 9 by water-cooled tube 22, be provided with on electric control box 23 top the first display screen 24, first pilot lamp 25, power switch 26, controller for vacuum pump 27, cooling-water pump controller 28, pressure electric machine controller 29, heating temperature control 30, heat-up time controller 31, electric control box 23 is connected with plasma discharge hot-pressed sintering furnace 1, vacuum pump 5, cooling-water pump 21 by the first wire 32.
Shown in Fig. 2, be magnesium alloy base neutron shield matrix material hot extrusion state graph, each position, annexation want correct, operate according to the order of sequence.
The extruding of magnesium alloy base neutron shield matrix material blank is carried out on hydraulic press, completes in heating, pressure process;
Hydraulic press is vertical, and the bottom of hydraulic press 33 is base 41, top is footstock 34, is provided with the second left socle 42, second right support 48 in base 41 bottom; The top of footstock 34 arranges hydraulic ram 35; Container 38 is put on base 41 top, container 38 outside is resistance heater 37, container 38 inner bottom part puts Extruding die 39, Extruding die 39 top is magnesium alloy base neutron shield matrix material blank 46, magnesium alloy base neutron shield matrix material blank 46 top is extruding punch 36, extruding punch 36 top is top briquetting 45, and top briquetting 45 top is traverser 44, and traverser 44 is connected by forcing spindle 43 with hydraulic ram 35; Extruding die 39 bottom connects discharge hole 40; Be hydraulic power unit 55 at hydraulic press 33 right part, hydraulic power unit 55 upper left quarter is provided with the first hydraulicefficiency pressure gauge 58, second hydraulicefficiency pressure gauge 59, and hydraulic power unit 55 is communicated with hydraulic ram 35 with oil outlet pipe 57 by oil inlet pipe 56; Hydraulic power unit 55 right part is electrical control cubicles 49, electrical control cubicles 49 is provided with second display screen 50, second pilot lamp 51, power-supply controller of electric 52, hydrauliccontroller 54, resistive heating controller 55, and electrical control cubicles 49 is connected with hydraulic power unit 55, resistance heater 37 by the second wire 47.
Shown in Fig. 3, be magnesium alloy base neutron shield matrix material square section displaing micro tissue topography figure, shown in figure: in magnesium alloy base neutron shield matrix material, B particle and Sm uniform particles are distributed in the middle of Mg alloying pellet, do not occur the agglomeration of B and Sm particle.
Shown in Fig. 4, magnesium alloy base neutron shield matrix material profile displaing micro tissue topography schemes, and shown in figure: in magnesium alloy base neutron shield matrix material, Mg alloying pellet particle under the effect of rolling pressure is elongated, be uniformly distributed between particle, interface cohesion is good.
Claims (3)
1. the preparation method of a magnesium alloy base neutron shield matrix material, it is characterized in that: the chemical substance material of use is: magnesium alloy powder, boron powder, samarium powder, dehydrated alcohol, graphite paper, sand paper, it is as follows that its combination prepares consumption: with gram, milliliter, millimeter for measure unit
Preparation method is as follows:
(1) cylindrical mold is prepared
Cylindrical mold graphite material makes, and mold cavity is of a size of Φ 40mm × 80mm, and mold cavity surfaceness is Ra 0.08-0.16 μm;
(2) dehumidifying, degassing processing magnesium alloy powder
Magnesium alloy powder is placed in quartz container, is then placed in vacuum furnace dry, drying temperature 50 DEG C, vacuum tightness≤2Pa, time of drying 30min;
(3) dehumidifying, degassing processing samarium powder
Samarium powder is placed in quartz container, is then placed in vacuum furnace dry, drying temperature 50 DEG C, vacuum tightness≤2Pa, time of drying 20min;
(4) dehumidifying, degassing processing boron powder
Boron powder is placed in quartz container, is then placed in vacuum furnace dry, drying temperature 100 DEG C, vacuum tightness≤2Pa, time of drying 20min;
(5) prepare burden
Batching is carried out in vacuum glove box, and vacuum glove box case pressure is-0.1mbar, water-content < 0.1ppm, oxygen level < 0.1ppm;
Take magnesium alloy powder 170g ± 0.01g, boron powder 20g ± 0.01g, samarium powder 10g ± 0.01g, be placed in ball grinder, ball sealer grinding jar;
Magnesium alloy powder: boron powder: samarium powder=17:2:1;
(6) ball mill mixing
The ball grinder of powder mix will be housed as on ball mill, ball milling mixes powder time 2h, drum's speed of rotation 1200rpm, and ball milling becomes mixing fine powders;
(7) feed
Ball grinder is placed in vacuum glove box, mixing fine powders is added in circular graphitic mould;
In mold cavity, place mould lower cushion block, at mould lower cushion block top placing graphite paper, place mixing fine powders on graphite paper top, at mixing fine powders top placing graphite paper, place mould seaming chuck on graphite paper top;
(8) hot pressed sintering of magnesium alloy base neutron shield matrix material blank
The hot pressed sintering of magnesium alloy base neutron shield matrix material carries out in plasma discharge hot-pressed sintering furnace, under vacuum conditions, heating, to complete in course of exerting pressure;
1. open plasma discharge hot-pressed sintering furnace, charged circular die is placed in lower electrode top, top electrode is pushed down cylindrical mold, and fixing;
Close plasma discharge hot-pressed sintering furnace;
2. open water device for cooling water pump, carries out outer water cycle cooling;
3. open vacuum pump, extract furnace air, make pressure≤2Pa in stove;
4. opening pressure motor, exerts pressure to mould, and exert pressure pressure 25kN;
5. open electric pulse heating device, Heating temperature, time were undertaken by four stages:
First stage: temperature is 20 DEG C ~ 350 DEG C, time 10min;
Subordinate phase: temperature is 350 DEG C ~ 450 DEG C, time 5min;
Phase III: temperature is 450 DEG C ~ 500 DEG C, time 5min;
Fourth stage: temperature is 500 DEG C of constant temperature insulations, time 10min;
6. after plasma discharge hot pressed sintering, close plasma discharge hot-pressed sintering furnace, stop heating, stop exerting pressure, cool to 25 DEG C with the furnace;
7. die sinking, opens plasma discharge hot-pressed sintering furnace, takes out graphite jig, opens graphite jig, takes out sintering block, is magnesium alloy base neutron shield matrix material blank;
(9) thermal treatment
The thermal treatment of magnesium alloy base neutron shield matrix material blank is carried out in resistance heading furnace, and cylinder blank is put into resistance heading furnace, and thermal treatment temp is 415 DEG C, and heat-up time is 24h;
Then 25 DEG C are cooled to the furnace;
(10) extruding of magnesium alloy base neutron shield matrix material
The extrusion molding of magnesium alloy base neutron shield matrix material is carried out on vertical hydraulic pressing machine, completes under heating, pressurization and Extruding die guide functions;
1. prepare extrusion mould, extrusion mould 4Cr5MoSiV1 hot-work die steel makes, and extrusion mould is made up of Extruding die, extruding punch and mould container;
2. extrusion mould cylindrical shell is placed on the worktable of vertical press, puts Extruding die in mould container inside, blank is placed in Extruding die, put extruding punch on blank top, resistance heater is set around mould container;
3. opening resistor well heater, heating mould and blank, Heating temperature is 350 DEG C ± 5 DEG C, constant temperature soaking time 60min;
4. open vertical press, extruding punch extrudes in Extruding die preformed body, and squeeze pressure is 100kN, is squeezed into rectangular plate, stops heating, make it naturally cool to 25 DEG C after extruding;
Die sinking after extruding, takes out rectangular plate, is magnesium alloy base neutron shield matrix material;
(11) polishing, sanding process
The magnesium alloy base neutron shield matrix material of preparation is placed on steel flat board, with sand papering periphery and surface, makes it clean;
(12) clean, with washes of absolute alcohol magnesium alloy base neutron shield composite material surface, make it clean;
(13) detect, analyze, characterize
The pattern of magnesium alloy base neutron shield matrix material of preparation, color and luster, chemical physics performance, mechanical property are detected, analyze, characterized;
The density test of material is carried out with Archimedes's drainage;
Hardness performance analysis is carried out with microhardness instrument;
Analysis on Microstructure is carried out with metaloscope instrument;
The test of shielding Neutron properties is carried out by Am-Be neutron source;
Conclusion: magnesium alloy base neutron shield matrix material is silvery white, material density reaches 99%, there is not samarium particle and boron particles agglomeration in material internal, samarium particle and boron particles are evenly distributed between magnesium alloy particles, between particle, interface cohesion is good, hardness reaches 140HV, and neutron-absorbing performance reaches 97%;
(14) store
The magnesium alloy base neutron shield matrix material soft material of preparation is packed, is stored in cleaning, dry environment, moistureproof, sun-proof, anti-acid-alkali salt to corrode, storing temp 20 DEG C, relative humidity≤10%.
2. the preparation method of a kind of magnesium alloy base neutron shield matrix material according to claim 1, is characterized in that:
The hot pressed sintering of magnesium alloy base neutron shield matrix material blank carries out in plasma discharge hot-pressed sintering furnace, under vacuum conditions, heating, to complete in course of exerting pressure;
Plasma discharge hot-pressed sintering furnace is vertical, the bottom of plasma discharge hot-pressed sintering furnace (1) is worktable (18), and worktable (18) bottom supports fixing by the first left socle (19), the first right support (20), be outer water cycle cooling tube (9) in plasma discharge hot-pressed sintering furnace outside, be furnace chamber (4) in plasma discharge hot-pressed sintering furnace (1) inside, furnace chamber (4) interior bottom is lower electrode (17), lower electrode (17) top is lower cushion block (15), lower cushion block (15) top is lower margin (14), lower margin (14) is stretched in cylindrical mold (12), lower margin (14) top is the first graphite paper (13), be magnesium alloy base neutron shield matrix material mixing fine powders (11) on the first graphite paper (13) top, be the second graphite paper (10) on magnesium alloy base neutron shield matrix material mixing fine powders (11) top, be seaming chuck (8) on the second graphite paper (10) top, be upper holder block (6) on seaming chuck (8) top, be top electrode (3) on upper holder block (6) top, on top electrode (3) top Bonding pressure motor (2), be electric control box (23) at the right part of plasma discharge hot-pressed sintering furnace (1), be worktable (18) in the bottom of plasma discharge hot-pressed sintering furnace (1), electric control box (23), be vacuum pump (5) at the lower left part of worktable (18), be communicated with furnace chamber (4) on vacuum pump (5) top by valve tube (7), be cooling water tank (16) at worktable (18) lower right section, cooling water tank (16) top is provided with cooling-water pump (21), and cooling-water pump (21) is communicated with outer water cycle cooling tube (9) by water-cooled tube (22), the first display screen (24), the first pilot lamp (5), power switch (26), controller for vacuum pump (27), cooling-water pump controller (28), pressure electric machine controller (29), heating temperature control (30), controller heat-up time (31) is provided with on electric control box (23) top, electric control box (23) is connected with plasma discharge hot-pressed sintering furnace (1), vacuum pump (5), cooling-water pump (21) by the first wire (32).
3. the preparation method of a kind of magnesium alloy base neutron shield matrix material according to claim 1, is characterized in that:
The extruding of magnesium alloy base neutron shield matrix material blank is carried out on hydraulic press, completes in heating, pressure process;
Hydraulic press is vertical, the bottom of hydraulic press (33) is base (41), top is footstock (34), is provided with the second left socle (42), the second right support (48) in base (41) bottom, the top of footstock (34) arranges hydraulic ram (35), container (38) is put on base (41) top, container (38) outside is resistance heater (37), container (38) inner bottom part puts Extruding die (39), Extruding die (39) top is magnesium alloy base neutron shield matrix material blank (46), magnesium alloy base neutron shield matrix material blank (46) top is extruding punch (36), extruding punch (36) top is top briquetting (45), top briquetting (45) top is traverser (44), traverser (44) is connected by forcing spindle (43) with hydraulic ram (35), Extruding die (39) bottom connects discharge hole (40), be hydraulic power unit (55) at pressing machine (33) right part, hydraulic power unit (55) upper left quarter is provided with the first hydraulicefficiency pressure gauge (58), the second hydraulicefficiency pressure gauge (59), and hydraulic power unit (55) is communicated with hydraulic ram (35) with oil outlet pipe (57) by oil inlet pipe (56), hydraulic power unit (55) right part is electrical control cubicles (49), electrical control cubicles (49) is provided with second display screen (50), the second pilot lamp (51), power-supply controller of electric (52), hydrauliccontroller (53), resistive heating controller (54), and electrical control cubicles (49) is connected with hydraulic power unit (55), resistance heater (37) by the second wire (47).
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| CN105568098A (en) * | 2016-03-14 | 2016-05-11 | 太原理工大学 | Preparation method for heat-resistant high-strength magnesium alloy material |
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| CN107400837A (en) * | 2017-07-31 | 2017-11-28 | 太原理工大学 | A kind of preparation method of nickle-based block non-crystaline amorphous metal |
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| CN113048781A (en) * | 2021-03-09 | 2021-06-29 | 王建生 | Vertical sintering furnace convenient to clean |
| CN113416873A (en) * | 2021-06-28 | 2021-09-21 | 晋中学院 | Rare earth magnesium alloy plate with high electromagnetic shielding effect and preparation method thereof |
| CN113580716A (en) * | 2021-07-13 | 2021-11-02 | 太原理工大学 | Preparation device and method of vacuum current-assisted high-strength plastic corrosion-resistant magnesium-aluminum laminated plate |
| CN117721338A (en) * | 2024-02-02 | 2024-03-19 | 有研工程技术研究院有限公司 | Radiation-resistant magnesium-based composite material and preparation method and application thereof |
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