CN106583708A - Preparation method of laminated gradient neutron absorbing material - Google Patents
Preparation method of laminated gradient neutron absorbing material Download PDFInfo
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- CN106583708A CN106583708A CN201611204683.8A CN201611204683A CN106583708A CN 106583708 A CN106583708 A CN 106583708A CN 201611204683 A CN201611204683 A CN 201611204683A CN 106583708 A CN106583708 A CN 106583708A
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- neutron absorber
- layered gradient
- absorber material
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000011358 absorbing material Substances 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 72
- 229910000838 Al alloy Inorganic materials 0.000 claims abstract description 36
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 34
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000005245 sintering Methods 0.000 claims abstract description 19
- 238000005096 rolling process Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000005098 hot rolling Methods 0.000 claims abstract description 6
- 230000008569 process Effects 0.000 claims abstract description 4
- 239000006096 absorbing agent Substances 0.000 claims description 52
- 239000000843 powder Substances 0.000 claims description 52
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 38
- 229910002804 graphite Inorganic materials 0.000 claims description 31
- 239000010439 graphite Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 238000002490 spark plasma sintering Methods 0.000 claims description 22
- 239000011812 mixed powder Substances 0.000 claims description 19
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 239000010936 titanium Substances 0.000 claims description 15
- 229910001938 gadolinium oxide Inorganic materials 0.000 claims description 14
- 229940075613 gadolinium oxide Drugs 0.000 claims description 14
- 238000000926 separation method Methods 0.000 claims description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 13
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000002585 base Substances 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 229910000831 Steel Inorganic materials 0.000 claims description 6
- 239000000470 constituent Substances 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 239000010959 steel Substances 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 230000003647 oxidation Effects 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000002828 fuel tank Substances 0.000 claims description 4
- 238000002955 isolation Methods 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 239000004576 sand Substances 0.000 claims description 4
- 238000003860 storage Methods 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000498 cooling water Substances 0.000 claims description 2
- 238000001514 detection method Methods 0.000 claims description 2
- 239000007770 graphite material Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims description 2
- 239000011777 magnesium Substances 0.000 claims description 2
- 238000005259 measurement Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 239000007779 soft material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 230000003746 surface roughness Effects 0.000 claims description 2
- 238000009864 tensile test Methods 0.000 claims description 2
- 229910000906 Bronze Inorganic materials 0.000 claims 1
- 239000004411 aluminium Substances 0.000 claims 1
- 239000010974 bronze Substances 0.000 claims 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract description 15
- 239000002131 composite material Substances 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000001192 hot extrusion Methods 0.000 abstract description 6
- 239000004033 plastic Substances 0.000 abstract description 4
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007547 defect Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 150000002910 rare earth metals Chemical class 0.000 description 2
- 229910052693 Europium Inorganic materials 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- -1 boron carbides Chemical class 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 229910001940 europium oxide Inorganic materials 0.000 description 1
- 229940075616 europium oxide Drugs 0.000 description 1
- AEBZCFFCDTZXHP-UHFFFAOYSA-N europium(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Eu+3].[Eu+3] AEBZCFFCDTZXHP-UHFFFAOYSA-N 0.000 description 1
- 229940059947 gadolinium Drugs 0.000 description 1
- UIWYJDYFSGRHKR-UHFFFAOYSA-N gadolinium atom Chemical compound [Gd] UIWYJDYFSGRHKR-UHFFFAOYSA-N 0.000 description 1
- 239000010720 hydraulic oil Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- KZUNJOHGWZRPMI-UHFFFAOYSA-N samarium atom Chemical compound [Sm] KZUNJOHGWZRPMI-UHFFFAOYSA-N 0.000 description 1
- 229910001954 samarium oxide Inorganic materials 0.000 description 1
- 229940075630 samarium oxide Drugs 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- B22F3/12—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
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
-
- 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
- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/02—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite layers
-
- 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
- B22F2003/185—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 by hot rolling, below sintering temperature
-
- 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
- B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
- B22F2003/208—Warm or hot extruding
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
-
- 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
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Powder Metallurgy (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a preparation method of a laminated gradient neutron absorbing material. To overcome the defect that plastic deformation of high-content boron carbide and rare earth oxide aluminum alloy-based composite materials is difficult, aluminum alloy is adopted as an outer layer material, the contents of boron carbide and rare earth oxide are gradually increased from the outer layer to the inner layer, a neutron absorbing material blank is prepared through the plasma discharge sintering technology, hot extrusion is carried out through a hydraulic press machine, and the laminated gradient neutron absorbing material is prepared in a hot rolling mode through a rolling mill. According to the preparation method, the process is advanced, data are accurate and detailed, the tensile strength of the prepared neutron absorbing material reaches 240 MPa, the elongation percentage of the prepared neutron absorbing material reaches 6.3%, the corrosion resistance of the prepared neutron absorbing material can be improved by 70%, the prepared neutron absorbing material can be used for nuclear protection, and the preparation method is an advanced method for preparing laminated gradient metal-based composite materials.
Description
Technical field
The present invention relates to a kind of preparation method of layered gradient neutron absorber material, belongs to the skill that non-ferrous metal is prepared and applied
Art field.
Background technology
Samarium, europium in boron and rare earth oxide in boron carbide, such as samarium oxide, europium oxide, gadolinium oxide, gadolinium element have
Big neutron absorption cross-section, and boron carbide and rare earth oxide are cheap, in being often applied in nuclear power station shielding material
Sub- absorber, shielding absorbs neutron；But because boron carbide and rare earth oxide are difficult to be prepared into sheet material, often by boron carbide and rare earth
Oxide is added in aluminium alloy and is prepared into aluminium alloy based composites.
Inside aluminium alloy based composites, only when boron carbide and rare earth oxide content are higher than critical value, ability
Meet shielding completely and absorb neutron；When the boron carbide and rare earth oxide of high-load is added to alloy matrix aluminum inside, due to carbon
Change boron and the boundary moisture performance between rare earth oxide and alloy matrix aluminum is poor, interface bond strength is low, causes composite
Cracking is produced in the plastic histories such as extruding, rolling, it is difficult to prepare the aluminium alloy of high-load boron carbide and rare earth oxide
Based composites.
The aluminum laminate alloy-based for sintering different boron carbides and rare earth oxide content using spark plasma sintering technology is answered
Condensation material blank, blank is prepared into layered gradient neutron absorber material, boron carbide and rare earth oxygen after hot extrusion and hot rolling
Compound content is reduced by center outer layers, and outermost layer is aluminium alloy；When spark plasma sintering prepares blank, sintering velocity is fast,
Blank inside number of plies range of choice width；Be conducive to the interface cohesion between boron carbide and rare earth oxide and alloy matrix aluminum；Base
After hot extrusion, material density is improved material, and sheet material is rolled into after extruding, is that a kind of practicable layered gradient for preparing is answered
The preparation method of condensation material.
The content of the invention
Goal of the invention
The purpose of the present invention is the applicable cases for high-load boron carbide and rare earth oxide aluminium alloy based composites, is adopted
Boron carbide and gadolinium oxide are neutron absorber, material, titanium valve and magnesium powder are additive based on aluminium alloy, by different component content
Mixed powder with spark plasma sintering technology sinter layered circular blank；Blank is after hot extrusion and hot rolling into core
Boron carbide and the layered gradient neutron absorber material that rare earth oxide content is high, outer layer content is low, to improve neutron absorber material
Shielding properties, reduce shielding material thickness and volume, with adapt to nuclear defence shielding needs.
Technical scheme
The chemical substance material that the present invention is used is：Al alloy powder, boron carbide powder, gadolinium oxide powder, titanium valve, magnesium powder, absolute ethyl alcohol,
Aluminium alloy plate, graphite paper, aquadag, it is as follows that its combination prepares consumption：With gram, milliliter, millimeter as measurement unit
Al alloy powder：6061Al 90g±0.01g
Boron carbide powder：B4C 20 g±0.01g
Gadolinium oxide powder：Gd2O3 3g±0.01g
Titanium valve：Ti 3g±0.01g
Magnesium powder：Mg 3g±0.01g
Absolute ethyl alcohol：C2H5OH 500mL±10 mL
Aluminium alloy plate：2 pieces of 90mm × 1.5mm × 90mm of 6061Al
Graphite paper：2 pieces of 90mm × 2mm × 90mm of C
Aquadag：C 200mL±10 mL
Preparation method is as follows
（1）Prepare cylindrical mold
Cylindrical mold with graphite material make, mold cavity surface roughness be Ra 0.08-0.16 m, mold cavity size
For Φ 30mm × 80mm；
（2）Prepare separation layer
Separation layer makes of aluminium alloy plate, and aluminium alloy plate is fabricated to into cylindrical shape, and one is Φ 20mm × 85mm, and another is
Φ15mm×85mm；
（3）Pre-oxidation treatment boron carbide powder
Boron carbide powder is placed in quartz container, being subsequently placed in heating furnace carries out pre-oxidation treatment, 450 DEG C of Pre oxidation,
Preoxidation time 30min；
（4）Dispensing
1. Al alloy powder 25.2g ± 0.01g, boron carbide powder 3g ± 0.01g, gadolinium oxide powder 0.6g ± 0.01g, titanium valve are weighed
0.3g ± 0.01g, magnesium powder 0.3g ± 0.01g is in being placed in ball grinder A and closed；
Al alloy powder：Boron carbide powder：Gadolinium oxide powder：Titanium valve：Magnesium powder=86:10:2:1:1；
2. Al alloy powder 19.8g ± 0.01g, boron carbide powder 9g ± 0.01g, gadolinium oxide powder 0.6g ± 0.01g, titanium valve are weighed
0.3g ± 0.01g, magnesium powder 0.3g ± 0.01g is in being placed in ball grinder B and closed；
Al alloy powder：Boron carbide powder：Gadolinium oxide powder：Titanium valve：Magnesium powder=66:30:2:1:1；
3. Al alloy powder 30g ± 0.01g are weighed；
（5）Ball milling mixes powder
Ball grinder A and B are respectively placed on ball mill, the mixed powder of ball milling is carried out respectively, the mixed powder revolution of ball milling is 300r/min, ball
The mill mixed powder time is 60min, into the quaternary mixed powder of two kinds of different constituent element contents after the mixed powder of ball milling；
（6）Charging
1. cylindrical mold is vertically arranged on steel flat board, lower cushion block is placed in into mould inner bottom part, in the laying of lower cushion block top
Graphite paper, the isolation of Φ 20mm × 85mm is placed in cylindrical mold die cavity, and between two parties, by Al alloy powder 30g ± 0.01g
Load between separation layer and cylindrical mold inwall, and be compacted；
2. the separation layer inside for the isolation of Φ 15mm × 85mm being placed on into Φ 20mm × 85mm is simultaneously placed in the middle, by ball grinder A
Quaternary mixed powder loads between separation layer, and is compacted；
3. the quaternary mixed powder in ball grinder B is loaded inside the separation layer of Φ 15mm × 85mm, and is compacted；
4. two separation layers of Φ 15mm × 85mm, Φ 20mm × 85mm are taken out, in mixed powder top placing graphite paper, in graphite
Place mould upper holder block in paper top；
（7）The blank sintering of layered gradient neutron absorber material
The blank sintering of layered gradient neutron absorber material is carried out in plasma discharge hot-pressed sintering furnace, is in vacuum ring
Under border, heating, complete in course of exerting pressure；
1. plasma discharge hot-pressed sintering furnace is opened, the graphite jig parallel vertical that will be equipped with stratiform mixed powder is moved in furnace chamber
Bottom electrode top, and graphite jig is compressed by Top electrode, and it is fixed, close fire door；
2. water-cooling system is opened, water circulation cooling is carried out, vavuum pump is opened, furnace air is extracted, pressure≤5Pa in stove is made；
3. Opening pressure motor, presses to mould, and applying pressure is 30MPa；
4. plasma discharge heater is opened, heating-up temperature, time are carried out by three stages；
First stage：Temperature is 20 DEG C～550 DEG C, time 10min；
Second stage：Temperature is 550 DEG C～590 DEG C, time 5min；
Phase III：Temperature is that 590 DEG C of constant temperature are incubated, time 10min；
5. after spark plasma sintering, spark plasma sintering stove is closed, stops heating, stop pressure, cool to≤200 with the furnace
℃
6. plasma discharge hot-pressed sintering furnace is opened, graphite jig is taken out, die sinking takes out sintering block, as in layered gradient
Sub- absorbing material blank；
（8）Grinding process
Layered gradient neutron absorber material blank is placed on steel flat board, with sand papering circumference and end face so as to clean；
Then washes of absolute alcohol is used so as to clean；
（9）The extruding of layered gradient neutron absorber material
The extrusion molding of layered gradient neutron absorber material is carried out on vertical press, is in heating, pressurization and extruding
Complete under die guide functions；
1. extrusion die is placed on press bench, and in Extruding die inwall lubricant aquadag is smeared；
2. cylinder blank is placed in Extruding die, blank pressure in extruding punch alignment die；
3. the heater on Opening pressure machine worktable, heats, 480 DEG C of heating-up temperature to the Extruding die equipped with blank,
Constant temperature is incubated 20min；
4. Opening pressure machine, is directed at extruding punch and is pressed, and blank is clamp-oned in die, layered gradient neutron absorber material
Blank；
（10）The rolling of layered gradient neutron absorber material
The rolling of layered gradient neutron absorber material is carried out on hot-rolling mill, is completed in a heated condition；
By the layered gradient neutron absorber material blank heating of extrusion molding to 480 DEG C, 3 passes, rolling reduction are carried out
For 70%, layered gradient neutron-absorbing plate shape material；
（11）Polishing, cleaning
The layered gradient neutron-absorbing plate shape material of rolling is placed on steel flat board, with the positive and negative surface of sand papering and periphery,
Clean it；Then cleaned with absolute ethyl alcohol so as to clean；
（12）Detection, analysis, sign
The pattern of the layered gradient neutron absorber material to preparing, mechanical property are detected, analyzed, characterized；
Analysis on Microstructure is carried out with metallographic microscope；
Tensile property analysis is carried out with universal tensile test instrument；
Conclusion：Layered gradient neutron absorber material is silver gray plate shape, and outside is aluminium alloy layer, internal for two layers of gradient layer, layer
Good with reference to compactness between layer, each constituent element in different layers is evenly distributed, and with good processability, tensile strength reaches
240MPa, up to 6.3%, anticorrosive energy can improve 70% to elongation；
（13）Storage
Layered gradient neutron-absorbing plate shape material to preparing is packed with soft material, is stored in cleaning, dry environment, to be prevented
Damp, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
Beneficial effect
The present invention has significantly advance compared with background technology, is for high-load boron carbide and rare earth oxide aluminium alloy
The drawbacks of based composites plastic deformation is difficult, adopts aluminium alloy for cladding material, by outer layers towards inner layers boron carbide and rare-earth oxidation
The mode that thing content gradually rises, using spark plasma sintering technology neutron absorber material blank is prepared, Jing hot extrusions and
Hot rolling, makes layered gradient neutron absorber material, and this preparation method technique is advanced, and data are accurately full and accurate, and the neutron of preparation is inhaled
Receive Tensile strength and reach 240MPa, up to 6.3%, corrosion resistance improves 70% to elongation percentage, can do the neutron-absorbing material of nuclear defence
Material is used, and is the advanced method for preparing layered gradient metal-base composites.
Description of the drawings
Fig. 1, layered gradient neutron absorber material sinter molding state diagram
Fig. 2, layered gradient neutron absorber material hot extrusion state diagram
Microstructure morphology after Fig. 3, the extruding of layered gradient neutron absorber material
Microstructure morphology after Fig. 4, the rolling of layered gradient neutron absorber material
Fig. 5, layered gradient neutron absorber material stress-strain curve
Shown in figure, list of numerals it is as follows：
1st, spark plasma sintering stove, 2, upper holder block, 3, Top electrode, the 4, first graphite paper, 5, interior water circulation cooling tube, 6, graphite
Mould, 7, lower cushion block, 8, bottom electrode, 9, workbench, 10, return pipe, 11, outlet pipe, 12, water pump, 13, water tank, 14, left
Frame, 15, pressure motor, 16, stratiform mixing fine powders, the 17, second graphite paper, 18, thermocouple, the 19, first display screen, 20, first
Electrical control cubicles, the 21, first indicator lamp, 22, pressure electric machine controller, 23, controller for vacuum pump, 24, pulse current controller, 25,
Power switch, the 26, first wire, the 27, second wire, 28, vacuum tube, 29, right support, 30, vavuum pump, 31, privates,
32nd, bracing frame, 33, hydraulic press, 34, footstock, 35, hydraulic jack, 36, extruding punch, 37, resistance heater, 38, extruding
Cylinder, 39, Extruding die, 40, discharge opening, 41, base, the 42, second left socle, 43, pressure axis, 44, mobile work platform, 45, on
Portion's briquetting, 46, layered gradient neutron absorber material sintering blank, 47, privates, the 48, second right support, 49, second is automatically controlled
Cabinet, 50, first pressure table, 51, second pressure table, 52, oil inlet pipe, 53, oil return pipe, the 54, second indicator lamp, 55, second shows
Screen, 56, power-supply controller of electric, 57, hydraulic controller, 58, resistance heating controller, 59, hydraulic oil container.
Specific embodiment
Below in conjunction with accompanying drawing, the present invention will be further described：
It is layered gradient neutron absorber material sinter molding state diagram shown in Fig. 1, each portion position, annexation are correct, according to quantity
Proportioning, sequentially operates.
The sinter molding of layered gradient neutron absorber material is carried out on spark plasma sintering stove, be heating,
Complete in vacuum, pressure, interior water circulation cooling procedure；
Spark plasma sintering stove is vertical, and on the top of workbench 9, inside is provided with interior water circulation to spark plasma sintering stove 1
Cooling water pipe 5, top is provided with pressure motor 15；The inside of spark plasma sintering stove 1 is provided with bottom electrode 8, the top of bottom electrode 8
For lower cushion block 7, the top of lower cushion block 7 is the second graphite paper 17, and stratiform mixing fine powders 16, stratiform are put in the top of the second graphite paper 17
The outside of mixing fine powders 16 is graphite jig 6, and the top of graphite jig 6 is provided with thermocouple 18, and the top of stratiform mixing fine powders 16 is the
One graphite paper 4, the top of the first graphite paper 4 is upper holder block 2, and the top of upper holder block 2 is Top electrode 3；The bottom of workbench 9 is provided with first
Left socle 14, the first right support 29, and connect bracing frame 32, water tank 13 is placed on the top of bracing frame 32, and the upper right quarter of water tank 13 is installed
There is water pump 12, spark plasma sintering stove 1 is connected with water pump 12 by outlet pipe 11, is connected with water tank 13 by return pipe 10；
The right part of water tank 13 is vavuum pump 30, and vavuum pump 30 is connected by vacuum tube 28 with spark plasma sintering stove 1；Plasma discharge
The right side of sintering furnace 1 be the first switch board 20, be provided with the first switch board 20 first display screen 19, the first indicator lamp 21,
Power switch 25, pressure electric machine controller 22, pulse current controller 24, controller for vacuum pump 23；First switch board 20 passes through
First wire 26, the second wire 27, privates 31 are connected with spark plasma sintering stove 1, vavuum pump 30, water pump 12.
It is layered gradient neutron absorber material squeezed state figure shown in Fig. 2, each portion position, annexation are correct, sequentially
Operation.
Hydraulic press is vertical, and it is footstock 34 that the bottom of hydraulic press 33 is base 41, top；Set in the bottom of base 41
There are the second left socle 42, the second right support 48；The top of footstock 34 arranges hydraulic jack 35；Recipient is put on the top of base 41
38, the outside of recipient 38 is resistance heater 37, and the inner bottom part of recipient 38 puts Extruding die 39, and the top of Extruding die 39 is layer
Shape gradient neutron absorber material blank 46, the top of layered gradient neutron absorber material blank 46 be extruding punch 36, extruding punch
36 tops are top briquetting 45, and the top of top briquetting 45 is mobile work platform 44, and mobile work platform 44 passes through with hydraulic jack 35
Pressure axis 43 connects；The bottom of Extruding die 39 connects discharge opening 40；The right part of hydraulic press 33 be the second switch board 49, second
It is fuel tank 59 that the upper left quarter of switch board 49 is provided with the first hydralic pressure gauge 50, the second hydralic pressure gauge 51, bottom, and fuel tank 59 passes through oil inlet pipe 52
Connect with oil return pipe 53 with hydraulic jack 35, the second switch board 49 is provided with second display screen 55, the second indicator lamp 54, power supply control
Device processed 56, hydraulic controller 57, resistance heating controller 58, the second switch board 49 is by privates 47 and resistance heater 37
Connection.
It is microstructure morphology after the extruding of layered gradient neutron absorber material, shown in figure shown in Fig. 3：Inhale in neutron
Receive and be well combined between material internal layer, the defects such as crackle and pore do not occur, be evenly distributed between each constituent element in layer inside, do not go out
Existing agglomeration.
It is microstructure morphology after the rolling of layered gradient neutron absorber material, shown in figure shown in Fig. 4：Through rolling
After, it is high-visible between layers, it is evenly distributed between each constituent element.
It is layered gradient neutron absorber material stress-strain curve, shown in figure shown in Fig. 5：Layered gradient neutron is inhaled
Receive material tensile strength reach 240MPa, elongation percentage up to 6.3%, with good plastic deformation ability.
Claims (3)
1. a kind of preparation method of layered gradient neutron absorber material, it is characterised in that：The chemical substance material for using is：Aluminium is closed
Bronze, boron carbide powder, gadolinium oxide powder, titanium valve, magnesium powder, absolute ethyl alcohol, aluminium alloy plate, graphite paper, aquadag, its combination prepares to use
Amount is as follows：With gram, milliliter, millimeter as measurement unit
Al alloy powder：6061Al 90g±0.01g
Boron carbide powder：B4C 20 g±0.01g
Gadolinium oxide powder：Gd2O3 3g±0.01g
Titanium valve：Ti 3g±0.01g
Magnesium powder：Mg 3g±0.01g
Absolute ethyl alcohol：C2H5OH 500mL±10 mL
Aluminium alloy plate：2 pieces of 90mm × 1.5mm × 90mm of 6061Al
Graphite paper：2 pieces of 90mm × 2mm × 90mm of C
Aquadag：C 200mL±10 mL
Preparation method is as follows：
（1）Prepare cylindrical mold
Cylindrical mold with graphite material make, mold cavity surface roughness be Ra 0.08-0.16 m, mold cavity size
For Φ 30mm × 80mm；
（2）Prepare separation layer
Separation layer makes of aluminium alloy plate, and aluminium alloy plate is fabricated to into cylindrical shape, and one is Φ 20mm × 85mm, and another is
Φ15mm×85mm；
（3）Pre-oxidation treatment boron carbide powder
Boron carbide powder is placed in quartz container, being subsequently placed in heating furnace carries out pre-oxidation treatment, 450 DEG C of Pre oxidation,
Preoxidation time 30min；
（4）Dispensing
1. Al alloy powder 25.2g ± 0.01g, boron carbide powder 3g ± 0.01g, gadolinium oxide powder 0.6g ± 0.01g, titanium valve are weighed
0.3g ± 0.01g, magnesium powder 0.3g ± 0.01g is in being placed in ball grinder A and closed；
Al alloy powder：Boron carbide powder：Gadolinium oxide powder：Titanium valve：Magnesium powder=86:10:2:1:1；
2. Al alloy powder 19.8g ± 0.01g, boron carbide powder 9g ± 0.01g, gadolinium oxide powder 0.6g ± 0.01g, titanium valve are weighed
0.3g ± 0.01g, magnesium powder 0.3g ± 0.01g is in being placed in ball grinder B and closed；
Al alloy powder：Boron carbide powder：Gadolinium oxide powder：Titanium valve：Magnesium powder=66:30:2:1:1；
3. Al alloy powder 30g ± 0.01g are weighed；
（5）Ball milling mixes powder
Ball grinder A and B are respectively placed on ball mill, the mixed powder of ball milling is carried out respectively, the mixed powder revolution of ball milling is 300r/min, ball
The mill mixed powder time is 60min, into the quaternary mixed powder of two kinds of different constituent element contents after the mixed powder of ball milling；
（6）Charging
1. cylindrical mold is vertically arranged on steel flat board, lower cushion block is placed in into mould inner bottom part, in the laying of lower cushion block top
Graphite paper, the isolation of Φ 20mm × 85mm is placed in cylindrical mold die cavity, and between two parties, by Al alloy powder 30g ± 0.01g
Load between separation layer and cylindrical mold inwall, and be compacted；
2. the separation layer inside for the isolation of Φ 15mm × 85mm being placed on into Φ 20mm × 85mm is simultaneously placed in the middle, by ball grinder A
Quaternary mixed powder loads between separation layer, and is compacted；
3. the quaternary mixed powder in ball grinder B is loaded inside the separation layer of Φ 15mm × 85mm, and is compacted；
4. two separation layers of Φ 15mm × 85mm, Φ 20mm × 85mm are taken out, in mixed powder top placing graphite paper, in graphite
Place mould upper holder block in paper top；
（7）The blank sintering of layered gradient neutron absorber material
The blank sintering of layered gradient neutron absorber material is carried out in plasma discharge hot-pressed sintering furnace, is in vacuum ring
Under border, heating, complete in course of exerting pressure；
1. plasma discharge hot-pressed sintering furnace is opened, the graphite jig parallel vertical that will be equipped with stratiform mixed powder is moved in furnace chamber
Bottom electrode top, and graphite jig is compressed by Top electrode, and it is fixed, close fire door；
2. water-cooling system is opened, water circulation cooling is carried out, vavuum pump is opened, furnace air is extracted, pressure≤5Pa in stove is made；
3. Opening pressure motor, presses to mould, and applying pressure is 30MPa；
4. plasma discharge heater is opened, heating-up temperature, time are carried out by three stages；
First stage：Temperature is 20 DEG C～550 DEG C, time 10min；
Second stage：Temperature is 550 DEG C～590 DEG C, time 5min；
Phase III：Temperature is that 590 DEG C of constant temperature are incubated, time 10min；
5. after spark plasma sintering, spark plasma sintering stove is closed, stops heating, stop pressure, cool to≤200 with the furnace
℃；
6. plasma discharge hot-pressed sintering furnace is opened, graphite jig is taken out, die sinking takes out sintering block, as in layered gradient
Sub- absorbing material blank；
（8）Grinding process
Layered gradient neutron absorber material blank is placed on steel flat board, with sand papering circumference and end face so as to clean；
Then washes of absolute alcohol is used so as to clean；
（9）The extruding of layered gradient neutron absorber material
The extrusion molding of layered gradient neutron absorber material is carried out on vertical press, is in heating, pressurization and extruding
Complete under die guide functions；
1. extrusion die is placed on press bench, and in Extruding die inwall lubricant aquadag is smeared；
2. cylinder blank is placed in Extruding die, blank pressure in extruding punch alignment die；
3. the heater on Opening pressure machine worktable, heats, 480 DEG C of heating-up temperature to the Extruding die equipped with blank,
Constant temperature is incubated 20min；
4. Opening pressure machine, is directed at extruding punch and is pressed, and blank is clamp-oned in die, layered gradient neutron absorber material
Blank；
（10）The rolling of layered gradient neutron absorber material
The rolling of layered gradient neutron absorber material is carried out on hot-rolling mill, is completed in a heated condition；
By the layered gradient neutron absorber material blank heating of extrusion molding to 480 DEG C, 3 passes, rolling reduction are carried out
For 70%, layered gradient neutron-absorbing plate shape material；
（11）Polishing, cleaning
The layered gradient neutron-absorbing plate shape material of rolling is placed on steel flat board, with the positive and negative surface of sand papering and periphery,
Clean it；Then cleaned with absolute ethyl alcohol so as to clean；
（12）Detection, analysis, sign
The pattern of the layered gradient neutron absorber material to preparing, mechanical property are detected, analyzed, characterized；
Analysis on Microstructure is carried out with metallographic microscope；
Tensile property analysis is carried out with universal tensile test instrument；
Conclusion：Layered gradient neutron absorber material is silver gray plate shape, and outside is aluminium alloy layer, internal for two layers of gradient layer, layer
Good with reference to compactness between layer, each constituent element in different layers is evenly distributed, and with good processability, tensile strength reaches
240MPa, up to 6.3%, anticorrosive energy can improve 70% to elongation；
（13）Storage
Layered gradient neutron-absorbing plate shape material to preparing is packed with soft material, is stored in cleaning, dry environment, to be prevented
Damp, sun-proof, anti-acid-alkali salt corrodes, 20 DEG C of storage temperature, relative humidity≤10%.
2. the preparation method of a kind of layered gradient neutron absorber material according to claim 1, it is characterised in that：Stratiform ladder
The sinter molding of degree neutron absorber material is carried out on spark plasma sintering stove, is in heating, vacuum, pressure, interior water
Complete during circulating cooling；
Spark plasma sintering stove is vertical, and on the top of workbench (9), inside is provided with interior water to spark plasma sintering stove (1)
Circulating cooling water pipe (5), top is provided with pressure motor (15)；The inside of spark plasma sintering stove (1) is provided with bottom electrode (8),
The top of bottom electrode (8) is lower cushion block (7), and the top of lower cushion block (7) is the second graphite paper (17), the second graphite paper (17) top
It is graphite jig (6) to put outside stratiform mixing fine powders (16), stratiform mixing fine powders (16), and graphite jig (6) top is provided with
Thermocouple (18), stratiform mixing fine powders (16) top is the first graphite paper (4), and the first graphite paper (4) top is upper holder block (2),
Upper holder block (2) top is Top electrode (3)；The bottom of workbench (9) is provided with the first left socle 14, the second right support 29, and connects
Water tank (13) is placed on bracing frame (32), bracing frame (32) top, and water tank (13) upper right quarter is provided with water pump (12), plasma discharge
Sintering furnace (1) is connected by outlet pipe (11) with water pump (12), is connected with water tank (13) by return pipe (10), water tank (13)
Right part is vavuum pump (30), and vavuum pump (30) is connected by vacuum tube (28) with spark plasma sintering stove (1)；Plasma discharge
The right side of sintering furnace (1) is the first switch board (20), and the first display screen (19), the first finger are provided with the first switch board (20)
Show lamp (21), power switch (25), pressure electric machine controller (22), pulse current controller (24), controller for vacuum pump (23)；
First switch board (20) is by the first wire (26), the second wire (27), privates (31) and spark plasma sintering stove
(1), vavuum pump (30), water pump (12) connection.
3. the preparation method of a kind of layered gradient neutron absorber material according to claim 1, it is characterised in that：It is described
The extruding of layered gradient neutron absorber material carry out on hydraulic press, complete in heating, pressure process；
Hydraulic press is vertical, and hydraulic press (33) bottom is base (41), top is footstock (34), under base (41)
Portion is provided with the second left socle (42), the second right support (48)；Footstock (34) top arranges hydraulic jack (35)；On base (41)
It is resistance heater (37) that portion is put outside recipient (38), recipient (38), and recipient (38) inner bottom part puts Extruding die
(39), Extruding die (39) top be layered gradient neutron absorber material blank (46), layered gradient neutron absorber material blank
(46) top is extruding punch (36), and extruding punch (36) top is top briquetting (45), and top briquetting (45) top is movement
Workbench (44), mobile work platform (44) is connected with hydraulic jack (35) by pressure axis (43)；Extruding die (39) bottom connects
Connect discharge opening (40)；It is the second switch board () 49 in hydraulic press (33) right part, the second switch board (49) upper left quarter is provided with
First hydralic pressure gauge (50), the second hydralic pressure gauge (51), bottom is fuel tank (59), and fuel tank (59) is by oil inlet pipe (52) and oil return pipe
(53) connect with hydraulic jack (35), the second switch board (49) is provided with second display screen (55), the second indicator lamp (54), power supply
Controller (56), hydraulic controller (57), resistance heating controller (58), the second switch board (49) by privates (47) with
Resistance heater (37) connects.
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