CN111250697A - Preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material - Google Patents
Preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material Download PDFInfo
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- CN111250697A CN111250697A CN202010096842.7A CN202010096842A CN111250697A CN 111250697 A CN111250697 A CN 111250697A CN 202010096842 A CN202010096842 A CN 202010096842A CN 111250697 A CN111250697 A CN 111250697A
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 229910001938 gadolinium oxide Inorganic materials 0.000 title claims abstract description 62
- 229940075613 gadolinium oxide Drugs 0.000 title claims abstract description 62
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000010937 tungsten Substances 0.000 title claims abstract description 54
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 46
- 230000005251 gamma ray Effects 0.000 title claims abstract description 44
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 38
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000000463 material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000011258 core-shell material Substances 0.000 title claims description 31
- 239000000843 powder Substances 0.000 claims description 65
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 38
- 239000010439 graphite Substances 0.000 claims description 37
- 229910002804 graphite Inorganic materials 0.000 claims description 37
- 238000003825 pressing Methods 0.000 claims description 28
- 238000005096 rolling process Methods 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000004140 cleaning Methods 0.000 claims description 20
- 238000000498 ball milling Methods 0.000 claims description 16
- 238000005245 sintering Methods 0.000 claims description 11
- 229910000838 Al alloy Inorganic materials 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- 239000011863 silicon-based powder Substances 0.000 claims description 8
- 229910001930 tungsten oxide Inorganic materials 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000004663 powder metallurgy Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 230000001050 lubricating effect Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 238000007780 powder milling Methods 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 4
- 230000005855 radiation Effects 0.000 abstract description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007769 metal material Substances 0.000 abstract description 2
- 239000002915 spent fuel radioactive waste Substances 0.000 abstract description 2
- 229910001080 W alloy Inorganic materials 0.000 description 10
- 239000007787 solid Substances 0.000 description 6
- 239000002131 composite material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 239000011159 matrix material Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052688 Gadolinium Inorganic materials 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 2
- 238000005461 lubrication Methods 0.000 description 2
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 2
- 239000011358 absorbing material Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000012809 cooling fluid Substances 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000010731 rolling oil Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007779 soft material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
-
- 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
-
- 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
- G21F1/08—Metals; Alloys; Cermets, i.e. sintered mixtures of ceramics and metals
- G21F1/085—Heavy metals or alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
Abstract
A preparation method of a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding material belongs to the technical field of preparation and application of non-ferrous metal materials, and aims to meet the protection requirement of nuclear power station spent fuel storage grillwork neutron radiation shielding.
Description
Technical Field
The invention belongs to the technical field of preparation and application of non-ferrous metal materials, and particularly relates to a preparation method of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material.
Background
The metal tungsten (W) has excellent gamma ray absorption capacity and is one of natural metal simple substances with higher density. Tungsten and its alloy are widely used in shielding materials, the tungsten alloy is a high specific gravity tungsten-based alloy, low in price, high in hardness and high in melting point, the tungsten content is not less than 90%, and nickel (Ni) and carbon (C) are mixed, so that the hardness and structural stability of the tungsten alloy can be enhanced. Therefore, tungsten alloy is one of the most potential gamma ray shielding materials in the future.
In conclusion, the neutron and gamma ray co-shielding material is designed by combining the rare earth oxide and the tungsten alloy, so that the neutron and gamma ray co-shielding material not only can absorb neutrons and gamma rays in the external environment, but also can effectively absorb secondary gamma rays generated by interaction of rare earth elements and neutrons. Tungsten alloy is a commonly used light and high-strength alloy, has better corrosion resistance and excellent radiation resistance, and is often used as a matrix material of a composite material. The rare earth oxide and the tungsten alloy are added into a tungsten alloy matrix to prepare a novel neutron and gamma ray co-shielding composite material which is a nuclear shielding structure material with great potential in the future.
Gadolinium (Gd) is the element with the highest thermal neutron absorption cross section in the applicable range, gadolinium oxide is low in cost, but gadolinium (Gd) can release secondary gamma rays while absorbing thermal neutrons; tungsten (W) is an excellent gamma-ray absorbing material.
Disclosure of Invention
The invention aims to provide a preparation method of a novel neutron and gamma ray co-shielding composite material, which takes tungsten alloy powder, aluminum alloy powder and gadolinium oxide powder as raw materials; degassing pretreatment, preparing a reinforcing phase, ball-milling mixed powder, pressing and rolling to prepare the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding plate.
The invention adopts the following technical scheme:
a preparation method of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material comprises the following steps:
first, preparation of the core-shell structure of the powder
Weighing gadolinium oxide powder and tungsten powder, placing the gadolinium oxide powder and the tungsten powder in a ball mill, and carrying out ball milling for 6 hours at the ball milling revolution of 800r/min to obtain tungsten/gadolinium oxide core-shell structure mixed fine powder;
second, making an open-close type mold
Adopt stainless steel material to make open-close type mould, the mould die cavity is the rectangle cavity, and the size is 30mm x 60mm, and die cavity surface roughness is: ra0.08-0.16 um;
thirdly, mixing powder and ball milling
Weighing aluminum alloy powder, silicon powder, boric acid and mixed fine powder with a tungsten/gadolinium oxide core-shell structure, placing the mixed fine powder in a quartz container, stirring the mixture into mixed fine powder A, putting the mixed fine powder A into a ball mill, carrying out ball milling for 120min at the ball milling revolution of 400r/min to obtain mixed fine powder B;
fourthly, the mould is filled
Vertically placing an open-close type die on a steel flat plate, placing a graphite cushion block at the bottom of a cavity of the open-close type die, placing first graphite paper on the graphite cushion block, placing mixed fine powder B on the first graphite paper, placing second graphite paper on the mixed fine powder B, and placing a graphite pressing block on the second graphite paper;
fifthly, powder metallurgy, sintering and blank making
Vertically moving the open-close type mold for mold loading into a workbench in a vacuum hot-pressing sintering furnace, vertically pressing a graphite pressing block on the open-close type mold by an upper pressing block of the vacuum hot-pressing sintering furnace and a pressure motor, and sealing;
starting a vacuum pump, and pumping air in the furnace to ensure that the pressure in the furnace is constant at 2 Pa;
starting a plasma discharge heater of the vacuum hot-pressing sintering furnace, and heating to 500 +/-1 ℃;
starting a pressure motor, and vertically applying pressure to a cavity of the open-close type mold, wherein the pressure intensity is 20MPa, and the constant-temperature pressure application time is 30 min; continuously heating to 585 +/-1 ℃, continuously applying pressure, wherein the pressure intensity is 40MPa, and applying pressure at constant temperature for 30 min;
after heating and pressing are finished, stopping heating and pressing, and cooling the opening-closing type die and the blank in the opening-closing type die to 25 ℃ along with the furnace;
closing the vacuum pump, opening the furnace and taking out the open-close type die; opening the mold, and taking out the blank, namely a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding absorption blank;
sixthly, cleaning, polishing and cleaning
Placing the blank on a steel flat plate, polishing the blank by using sand paper, then cleaning by using absolute ethyl alcohol, and drying in the air after cleaning;
seventh, heating and preserving heat
Placing the cleaned blank in a heat treatment furnace, heating and preserving heat at 500 ℃, and keeping the temperature constant;
eighth step of rolling
Placing the heated blank between an upper roller and a lower roller of a rolling mill, rolling from left to right in the rolling direction, wherein the rotation direction of the upper roller is anticlockwise rotation, and the rotation direction of the lower roller is clockwise rotation;
the rotating speed of the upper roller and the lower roller is 10 r/min; the rolling pass is six; forming a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate after rolling;
ninth, cleaning
And cleaning the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate with absolute ethyl alcohol, and drying after cleaning.
In the first step, the mass of the gadolinium oxide powder and the tungsten powder is 7 +/-0.01 g and 28 +/-0.01 g respectively.
In the third step, the mass of the aluminum alloy powder, the mass of the silicon powder, the mass of the boric acid and the mass of the tungsten/gadolinium oxide core-shell structure mixed fine powder are respectively 100 +/-0.01 g, 1.44 +/-0.01 g, 0.72 +/-0.01 g and 35 +/-0.01 g.
And in the second step, the opening-closing type die is rectangular, and four vertex angles of the opening-closing type die are assembled and fixed through the first opening-closing frame, the second opening-closing frame, the third opening-closing frame and the fourth opening-closing frame respectively.
And in the eighth step, the rolling mill is provided with a finishing roll, an inlet side cooling unit is arranged on the inlet side of the finishing roll, an outlet side cooling unit is arranged on the outlet side of the finishing roll, a wiper device in contact with the surface of the finishing roll is arranged on the lower portion of the inlet side cooling unit, a lubricating unit is arranged on the upper portion of the wiper device, and the wiper device comprises a cooling nozzle and a cooling pipeline.
Gd is prepared by coating a layer of metal tungsten on the surface of gadolinium oxide particles2O3The W micro-core-shell particle can absorb incident gamma rays and secondary gamma rays simultaneously. Then Gd is added2O3the/W core-shell particles are uniformly added into a tungsten (Al) matrix to prepare Gd2O3the/W/Al core-shell structure composite material (GWAC material for short) achieves the purpose of shielding neutrons and gamma rays together. Meanwhile, W14Al86 formed in situ at the tungsten interface strengthens interface connection, and the hard core-shell particles form dispersion strengthening to the composite material. The GWAC nuclear shell common shielding material has double functions and excellent structure, and realizes the design of structure/function integration.
The invention has the following beneficial effects:
the invention has obvious advancement compared with the background, is directed against the demand of neutron radiation shielding protection of a spent fuel storage grillwork of a nuclear power station, prepare gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate, adopt tungsten powder, gadolinium oxide powder, aluminum alloy powder to mix, make the blank through powder metallurgy, roll the blank, make gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate with high density, the neutron absorption plate is silvery white, neutron absorptivity reaches 96%, gadolinium oxide distributes evenly, the granule is connected with the basal body closely, the tensile strength reaches 300MPa, the elongation is 4%, the preparation method is advanced and rational, the parameter is accurate and real, it is the advanced method for preparing gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate.
Drawings
FIG. 1 is a diagram of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material mixed fine powder filling state;
FIG. 2 is a schematic structural diagram of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding plate rolling device;
FIG. 3 is a microstructure morphology of a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material prepared by the present invention;
FIG. 4 is a schematic diagram of tensile properties of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material prepared by the present invention;
wherein: 1-a mould cavity; 2-pressing graphite blocks; 3-a graphite cushion block; 4-a first opening and closing frame; 5-a second opening and closing frame; 6-a third opening and closing frame; 7-a fourth split frame; 8-opening and closing type mould; 9-gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material mixed fine powder; 10-first graphite paper; 11-second graphite paper; 12-core-shell structure; 13-inlet side cooling unit; 14-an outlet-side cooling unit; 15-finishing roll; 16-a cooling nozzle; 17-a wiper device; 18-a lubrication unit; 19-a cooling conduit; and 20-blank.
Detailed Description
The chemical substances used in the invention are: the preparation method comprises the following steps of preparing tungsten alloy powder, aluminum alloy powder, gadolinium oxide powder, silicon powder, absolute ethyl alcohol, boric acid and graphite paper, wherein the preparation dosage is as follows: measured in grams, milliliters and millimeters.
Tungsten alloy powder: w, 28g +/-0.01 g; aluminum alloy powder: 6061Al, 100g +/-0.01 g; gadolinium oxide powder: gd (Gd)2O37g +/-0.01 g; silicon powder: si, 1.44g +/-0.01 g; anhydrous ethanol: c2H5OH 1000mL +/-10 mL; boric acid: b is2O•3H2O, 0.72g +/-0.01 g; graphite paper: c, 30mm by 1mm, 4 pieces.
(1) The chemical materials required for preparation are selected and subjected to quality purity control.
Tungsten powder: solid powder, 99.9%; aluminum alloy powder: solid powder, 99.5%; silicon powder: 99.5% of solid crystal, gadolinium oxide powder: solid powder, 99.9%; anhydrous ethanol: liquid, 99.7%; boric acid: solid crystals, 99.5%; graphite paper: solid paper, 99.5%.
(2) Preparation of core-shell structures of powders
Weighing 7g +/-0.01 g of gadolinium oxide powder and 28g +/-0.01 g of tungsten powder, placing the gadolinium oxide powder and the tungsten powder in a ball mill, and carrying out ball milling for 6 hours at the ball milling revolution of 800r/min to obtain tungsten/gadolinium oxide core-shell structure mixed fine powder;
(3) manufacturing open-close type die
Adopt stainless steel material to make open-close type mould, the mould die cavity is the rectangle cavity, and the size is 30mm x 60mm, and die cavity surface roughness is: ra0.08-0.16 um;
(4) powder mixing ball mill
Weighing 100g +/-0.01 g of aluminum alloy powder, 1.44g +/-0.01 g of silicon powder, 0.72g +/-0.01 g of boric acid and 35g +/-0.01 g of tungsten/gadolinium oxide core-shell structure mixed fine powder, placing the mixture in a quartz container, and stirring the mixture into mixed fine powder; putting the mixed fine powder into a ball mill, and carrying out ball milling, wherein the ball milling revolution is 400r/min, and the ball milling time is 120min, so as to obtain mixed fine powder;
(5) die filling
Vertically placing an open-close type die on a steel flat plate, placing a graphite cushion block at the bottom of a cavity of the open-close type die, placing first graphite paper on the upper part of the graphite cushion block, placing mixed fine powder on the upper part of the first graphite paper, placing second graphite paper on the upper part of the mixed fine powder, and placing a graphite pressing block on the upper part of the second graphite paper;
(6) sintered blank made by powder metallurgy
① vertically moving the open-close type mold into the vacuum hot-pressing sintering furnace, vertically pressing the graphite pressing block on the open-close type mold by the upper pressing block of the vacuum hot-pressing sintering furnace and the pressure motor, and sealing;
② starting a vacuum pump to pump air in the furnace to make the pressure in the furnace constant at 2 Pa;
③ starting a plasma discharge heater of the vacuum hot-pressing sintering furnace, and heating to 500 +/-1 ℃;
starting a pressure motor, vertically applying pressure to the open-close type die cavity, wherein the pressure intensity is 20MPa, and the constant-temperature pressure application time is 30 min; continuously heating to 585 +/-1 ℃, continuously applying pressure, wherein the pressure intensity is 40MPa, and applying pressure at constant temperature for 30 min;
④ stopping heating and pressing, and furnace cooling the open-close type die and the blank therein to 25 deg.C;
⑤ closing the vacuum pump, opening the furnace to take out the open-close type mold, opening the mold, taking out the blank, namely gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding absorption blank;
(7) cleaning, polishing and cleaning
Placing the blank on a steel flat plate, and polishing each part of the blank by using abrasive paper; then absolute ethyl alcohol is used for cleaning, and the air is dried after cleaning;
(8) heating and heat preservation
Placing the blank in a heat treatment furnace, heating and preserving heat at the heating temperature of 500 ℃ and keeping the temperature;
(9) rolling of
Placing the heated blank between an upper roller and a lower roller of a rolling mill, rolling from left to right in the rolling direction, wherein the rotation direction of the upper roller is anticlockwise rotation, and the rotation direction of the lower roller is clockwise rotation;
the rotating speed of the upper roller and the lower roller is 10 r/min;
the rolling pass is six;
forming a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate after rolling;
(10) cleaning of
Cleaning the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate with absolute ethyl alcohol, and drying the cleaned nuclear shell common shielding plate;
(11) detection, analysis, characterization
Detecting, analyzing and representing the color, appearance, metallographic structure, microhardness and neutron absorption rate of the gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding plate;
detecting and analyzing the neutron absorptivity by using a neutron fluence rate instrument;
carrying out metallographic structure and microstructure morphology analysis by using an electron microscope and a scanning electron microscope;
carrying out microhardness analysis by using a microhardness instrument;
analyzing the bending strength and the tensile strength by using a universal testing machine;
(12) storage of
The prepared gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate is packaged by a soft material and stored in a dry and clean environment, and the plate needs to be waterproof, moistureproof and acid-base salt corrosion resistant, and has the storage temperature of 20 ℃ and the relative humidity of 10%.
As shown in fig. 1, the state diagram of the die filling of the mixed fine powder of the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material is shown, an open-close type die 8 is rectangular and is assembled and fixed by a first open-close frame 4, a second open-close frame 5, a third open-close frame 6 and a fourth open-close frame 7, a die cavity 1 is arranged inside the open-close type die 8, a graphite cushion block 3 is arranged at the bottom inside the die cavity 1, first graphite paper 10 is arranged on the upper portion of the graphite cushion block 3, mixed fine powder 9 of the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material is arranged on the upper portion of the first graphite paper 10, second graphite paper 11 is arranged on the upper portion of the mixed fine powder 9 of the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material, and graphite press block 2 is.
As shown in FIG. 2, the position and connection relationship of each part of a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding plate rolling device need to be rolled correctly and sequentially.
An inlet-side cooling unit 13 is provided on the inlet side of the finishing roll 15 to supply cooling water to the finishing roll 15, and an outlet-side cooling unit 14 is provided on the outlet side of the finishing roll 15 to supply cooling water to the finishing roll 15. Wherein a wiper device 17 provided at a lower portion of the inlet-side cooling unit 13 contacts a surface of the finishing roll 15. The upper part of the wiper device 17 may be provided with a lubrication unit 18 for supplying rolling oil and air. And, the wiper device 17 includes: cooling nozzles 16 and cooling ducts 19 supply cooling fluid to the material at different locations.
As shown in fig. 3, a microstructure morphology of a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material is shown in the figure: it can be seen that the gadolinium oxide/tungsten core-shell particles are uniformly and alternately distributed in a net shape on the aluminum matrix.
As shown in fig. 4, a schematic drawing of tensile properties of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material is shown in the drawing: the tensile strength reaches 300MPa, and the elongation is 4%, which shows that the prepared gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding material has good mechanical properties.
Claims (5)
1. A preparation method of a gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material is characterized by comprising the following steps: the method comprises the following steps:
first, preparation of the core-shell structure of the powder
Weighing gadolinium oxide powder and tungsten powder, placing the gadolinium oxide powder and the tungsten powder in a ball mill, and carrying out ball milling for 6 hours at the ball milling revolution of 800r/min to obtain tungsten/gadolinium oxide core-shell structure mixed fine powder;
second, making an open-close type mold
Adopt stainless steel material to make open-close type mould, the mould die cavity is the rectangle cavity, and the size is 30mm x 60mm, and die cavity surface roughness is: ra0.08-0.16 um;
thirdly, mixing powder and ball milling
Weighing aluminum alloy powder, silicon powder, boric acid and mixed fine powder with a tungsten/gadolinium oxide core-shell structure, placing the mixed fine powder in a quartz container, stirring the mixture into mixed fine powder A, putting the mixed fine powder A into a ball mill, carrying out ball milling for 120min at the ball milling revolution of 400r/min to obtain mixed fine powder B;
fourthly, the mould is filled
Vertically placing an open-close type die on a steel flat plate, placing a graphite cushion block at the bottom of a cavity of the open-close type die, placing first graphite paper on the graphite cushion block, placing mixed fine powder B on the first graphite paper, placing second graphite paper on the mixed fine powder B, and placing a graphite pressing block on the second graphite paper;
fifthly, powder metallurgy, sintering and blank making
Vertically moving the open-close type mold for mold loading into a workbench in a vacuum hot-pressing sintering furnace, vertically pressing a graphite pressing block on the open-close type mold by an upper pressing block of the vacuum hot-pressing sintering furnace and a pressure motor, and sealing;
starting a vacuum pump, and pumping air in the furnace to ensure that the pressure in the furnace is constant at 2 Pa;
starting a plasma discharge heater of the vacuum hot-pressing sintering furnace, and heating to 500 +/-1 ℃;
starting a pressure motor, and vertically applying pressure to a cavity of the open-close type mold, wherein the pressure intensity is 20MPa, and the constant-temperature pressure application time is 30 min; continuously heating to 585 +/-1 ℃, continuously applying pressure, wherein the pressure intensity is 40MPa, and applying pressure at constant temperature for 30 min;
after heating and pressing are finished, stopping heating and pressing, and cooling the opening-closing type die and the blank in the opening-closing type die to 25 ℃ along with the furnace;
closing the vacuum pump, opening the furnace and taking out the open-close type die; opening the mold, and taking out the blank, namely a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell co-shielding absorption blank;
sixthly, cleaning, polishing and cleaning
Placing the blank on a steel flat plate, polishing the blank by using sand paper, then cleaning by using absolute ethyl alcohol, and drying in the air after cleaning;
seventh, heating and preserving heat
Placing the cleaned blank in a heat treatment furnace, heating and preserving heat at 500 ℃, and keeping the temperature constant;
eighth step of rolling
Placing the heated blank between an upper roller and a lower roller of a rolling mill, rolling from left to right in the rolling direction, wherein the rotation direction of the upper roller is anticlockwise rotation, and the rotation direction of the lower roller is clockwise rotation;
the rotating speed of the upper roller and the lower roller is 10 r/min; the rolling pass is six; forming a gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate after rolling;
ninth, cleaning
And cleaning the gadolinium oxide/tungsten/aluminum neutron and gamma ray nuclear shell common shielding plate with absolute ethyl alcohol, and drying after cleaning.
2. The preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material according to claim 1, wherein the preparation method comprises the following steps: in the first step, the mass of the gadolinium oxide powder and the tungsten powder is 7 +/-0.01 g and 28 +/-0.01 g respectively.
3. The preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material according to claim 1, wherein the preparation method comprises the following steps: in the third step, the mass of the aluminum alloy powder, the mass of the silicon powder, the mass of the boric acid and the mass of the tungsten/gadolinium oxide core-shell structure mixed fine powder are respectively 100 +/-0.01 g, 1.44 +/-0.01 g, 0.72 +/-0.01 g and 35 +/-0.01 g.
4. The preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material according to claim 1, wherein the preparation method comprises the following steps: and in the second step, the opening-closing type die is rectangular, and four vertex angles of the opening-closing type die are assembled and fixed through the first opening-closing frame, the second opening-closing frame, the third opening-closing frame and the fourth opening-closing frame respectively.
5. The preparation method of gadolinium oxide/tungsten/aluminum neutron and gamma ray core-shell co-shielding material according to claim 1, wherein the preparation method comprises the following steps: and in the eighth step, the rolling mill is provided with a finishing roll, an inlet side cooling unit is arranged on the inlet side of the finishing roll, an outlet side cooling unit is arranged on the outlet side of the finishing roll, a wiper device in contact with the surface of the finishing roll is arranged on the lower portion of the inlet side cooling unit, a lubricating unit is arranged on the upper portion of the wiper device, and the wiper device comprises a cooling nozzle and a cooling pipeline.
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