CN105950897B - A kind of preparation method of copper-based neutron absorber material - Google Patents
A kind of preparation method of copper-based neutron absorber material Download PDFInfo
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- CN105950897B CN105950897B CN201610307340.8A CN201610307340A CN105950897B CN 105950897 B CN105950897 B CN 105950897B CN 201610307340 A CN201610307340 A CN 201610307340A CN 105950897 B CN105950897 B CN 105950897B
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- copper
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- neutron absorber
- graphite
- absorber material
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- 239000000463 material Substances 0.000 title claims abstract description 61
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 50
- 239000010949 copper Substances 0.000 title claims abstract description 50
- 239000006096 absorbing agent Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000010439 graphite Substances 0.000 claims abstract description 39
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 39
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 26
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000005245 sintering Methods 0.000 claims abstract description 24
- 239000002245 particle Substances 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000005452 bending Methods 0.000 claims abstract description 10
- 239000011812 mixed powder Substances 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 244000137852 Petrea volubilis Species 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 5
- 239000010432 diamond Substances 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 4
- 238000004140 cleaning Methods 0.000 claims abstract description 3
- 238000003825 pressing Methods 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 229910052796 boron Inorganic materials 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 7
- 239000000498 cooling water Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000004826 seaming Methods 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- 230000005684 electric field Effects 0.000 claims description 4
- 238000012876 topography Methods 0.000 claims description 4
- 238000005054 agglomeration Methods 0.000 claims description 3
- 230000002776 aggregation Effects 0.000 claims description 3
- 230000002745 absorbent Effects 0.000 claims description 2
- 239000002250 absorbent Substances 0.000 claims description 2
- 238000000498 ball milling Methods 0.000 claims description 2
- -1 boron carbides Chemical class 0.000 claims description 2
- 230000008859 change Effects 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000007689 inspection Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 claims description 2
- 239000002932 luster Substances 0.000 claims description 2
- 238000005088 metallography Methods 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 230000000704 physical effect Effects 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 238000005498 polishing Methods 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 230000002000 scavenging effect Effects 0.000 claims description 2
- 238000009864 tensile test Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910000712 Boron steel Inorganic materials 0.000 description 2
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 239000002915 spent fuel radioactive waste Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 206010020843 Hyperthermia Diseases 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000036031 hyperthermia Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
-
- 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
-
- 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
- B22F3/10—Sintering only
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
- C22C32/0057—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides based on B4C
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C21/00—Apparatus or processes specially adapted to the manufacture of reactors or parts thereof
- G21C21/18—Manufacture of control elements covered by group G21C7/00
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21C—NUCLEAR REACTORS
- G21C7/00—Control of nuclear reaction
- G21C7/06—Control of nuclear reaction by application of neutron-absorbing material, i.e. material with absorption cross-section very much in excess of reflection cross-section
- G21C7/24—Selection of substances for use as neutron-absorbing material
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
Abstract
The invention discloses a kind of preparation method of copper-based neutron absorber material, specifically applying pulse current to mixed-powder material using discharge plasma sintering technique makes to produce Joule heat and point discharge plasma between particle, makes to be partially melting to form metallurgical binding connection between particle；Used chemical material mainly includes during preparation：Copper powder, boron carbide powder, absolute ethyl alcohol, hydrochloric acid, hydrofluoric acid, deionized water, graphite paper, sand paper, diamond paste, preparation include：Pre-process copper powder, pretreatment boron carbide powder, claim with steps such as raw material, ball mill mixing, filling powder, pre-pressing die, discharge plasma sintering preparation process, cleaning sample surfaces, detection and analysis samples.Obtained copper-based neutron absorber material consistency is up to more than 99%, and copper-based neutron absorber material inside boron carbide Dispersed precipitate, bending strength is up to 350 ± 5MPa, and neutron-absorbing performance is up to 98%.
Description
Technical field
Present invention is a kind of preparation method of copper-based neutron absorber material, belongs to material processing preparation and application technology
Field.
Background technology
Neutron absorber material is widely used in nuclear industry, and currently used neutron absorber material is mainly that some have height
Thermal neutron and the metal in epithermal absorption section, it is nonmetallic, and its compound, such as conventional element boron, cadmium, silver etc..
Silver is not because expensive be generally made neutron absorber material and control rod use is often made.Although cadmium is with excellent neutron
Absorbent properties, but because its reserves is few, price is high and has toxicity, thus is gradually eliminated in recent decades.Boron is nature
The element of rich reserves, natural boron have two kinds of stable isotope B10And B11, that boron element has neutron absorption is B10（B10
Thermal neutron absorption cross section be 3837b, and 1/V absorbing rules can be obeyed in the range of wider neutron energy；B11Thermal neutron
Absorption cross-section only has 0.005b）.After boron absorbs neutron, soft γ photons are only produced（About 0.5MeV）With the α grains being easier to be absorbed by
Son, without big remaining artificial radioactivity, thus nuclear reactor is frequently with the material containing boron element（Such as B4C）In absorbing
Son.At present, the more ripe neutron absorber material of application has aluminum-based boron carbide, boron steel etc..Aluminum-based boron carbide material is due to its base
Body is aluminium and aluminium alloy thus is not resistant to high temperature and some corrosive atmospheres；Though boron steel heat resisting temperature it is higher by
In boron, solid solubility is very low in steel, and iron boron phase（Fe2B、FeB）It can be separated out on ferrite grain boundaries so as to significantly reduce matrix
Processing characteristics and mechanical property.
The content of the invention
In order to solve problems of the prior art, the present invention is for the purpose of meeting the needs of nuclear industry, there is provided one
The preparation method of the copper-based neutron absorber material of kind.
Technical scheme
The technical solution adopted by the present invention is：A kind of preparation method of copper-based neutron absorber material, using plasma discharging
Sintering technology, which applies pulse current to mixed-powder material, to be made to produce Joule heat and point discharge plasma between particle, is made
Metallurgical binding connection is partially melting to form between particle；Used chemical material is：Copper powder, boron carbide powder, absolute ethyl alcohol, salt
Acid, hydrofluoric acid, deionized water, graphite paper, sand paper, diamond paste, its dosage unit are：Gram, milliliter, millimeter（Below）
Copper powder：Cu50.066g±0.01g
Boron carbide powder：B4C6.194g±0.01g
Absolute ethyl alcohol：C2H5OH200mL±5mL
Hydrochloric acid：HCl15mL±5mL
Hydrofluoric acid：HF200mL±5mL
Deionized water：H2O500mL±5mL
Graphite paper：C
Sand paper：SiC400#
Diamond paste：C1.5mL
Preparation process is as follows：
(1) copper powder is pre-processed
Copper powder is placed in progress drying and processing 1h, 100 DEG C for the treatment of temperature in vacuum drying oven；
(2) boron carbide powder is pre-processed
1. boron carbide powder is put into pickling processes 0.5h in hydrofluoric acid；
2. boron carbide powder is taken out and rinsed repeatedly with deionized water to solution in neutrality；
3. boron carbide is placed in drying and processing 2h in drying baker, 300 DEG C for the treatment of temperature；
(3) claim to match somebody with somebody raw material
Weigh the laggard luggage of powder in vacuum glove box to match somebody with somebody, to avoid powder from aoxidizing, by the volume ratio of boron carbide and copper
For 3:7 ratios are matched, and weigh 6.194 ± 0.001g boron carbides and 50.066 ± 0.001g copper powders load ball grinder in the lump
In, it is put into zirconia ball sealing；
(4) ball mill mixing
It is 200rpm, ball milling 60min that the ball grinder assembled, which is installed to adjustment of rotational speed on ball mill,；
(5) powder is loaded
Four a diameter of 30mm of clip graphite paper disk, wherein two panels are previously charged into mold bottom compacting, in vacuum hand
In casing：Ball grinder is opened, the mixed powder mixed is fitted into mould, other two panels graphite paper is finally placed in mixing
Above powder, seaming chuck is pressed, the graphite jig for installing mixed powder is taken out from vacuum glove box；
(6) pre-pressing die
Graphite jig equipped with mixed powder is put into pre-molding on forcing press, pressure 20MPa, time 5min, so that
Mixed powder is compact formed；
(7) discharge plasma sintering preparation process
1. open control device and inspection apparatus；
2. set heating schedule and pressurization parameter：From room temperature to 400 DEG C, time 5min；400 DEG C -600 DEG C, time 5min；
600 DEG C -650 DEG C, time 2min；650 DEG C of insulation 5min；
3. the graphite jig pressed in advance is put into body of heater, and is accommodated and consolidated with push-down head, in discharge plasma sintering
In stove, graphite pressure head is provided with, pressure sensor is set above graphite pressure head, for detecting pressure of the graphite pressure head to graphite jig
Power situation, it is 40MPa to the pressure of graphite jig to set discharge plasma sintering furnace pressure head；
4. closing fire door, and vavuum pump is opened, make vacuum≤10-1Pa；
5. opening heating schedule, while pass through situation in peephole continuous observation stove；
6. heating terminates, cool down, blow-on, take out sample；
(8) sample surfaces are cleaned
The graphite of sample surfaces remaining is polished off with sand paper, absolute alcohol cleaning sample is used after polishing；
(9) sample is tested and analyzed
To the surface topography of obtained copper-based neutron absorber material, physical property, micro-nano mechanical property, mechanics of bending
Energy, neutron-absorbing performance are tested and analyzed and characterized：
Copper-based neutron absorber material consistency is measured using Archimedes's drainage；
Using the copper-based neutron absorber material microscopic appearance of metallography microscope sem observation；
Using scanning electron microscopic observation microstructure and fracture apperance；
Copper-based neutron absorber material microcell consistency and elasticity modulus is measured using nano-hardness tester；
The sliding and bending deformation of copper-based neutron absorber material is tested using universal tensile testing machine；
The neutron-absorbing performance of copper-based neutron absorber material is tested using NEUTRON EMISSION instrument；
Conclusion：Copper-based neutron absorber material appearance color is yellowish orange, and metallic luster is presented, consistency up to more than 99%,
Boron carbide Dispersed precipitate inside copper-based neutron absorber material, does not occur a large amount of agglomerations and is combined between particle and matrix
Well, bending strength is up to 350 ± 5MPa, and neutron-absorbing performance is up to 98%.
The present invention, with the actual demand of advanced technology combination nuclear industry, is used using copper as base for current techniques background
Body, boron carbide are that neutron absorber combination discharge plasma sintering technique is prepared with excellent mechanical property, high thermal conductivity,
The neutron absorber material that can be applied to more extensive more harsh environment of high neutron absorption performance.Using discharge plasma sintering skill
Art, in electric field, under the comprehensive function in temperature field and the field of force, make the uniform disperse of boron carbide particles in Copper substrate, vacuum bar
Material oxidation can be effectively prevented under part, impulse electric field makes to produce localized hyperthermia and fusing material surface between particle, so as to
So that between particle combine it is even closer, heat with pressurize in the presence of material density further improve.
Material bending strength is up to 350 ± 5MPa, and up to 98%, even particle distribution is tightly combined neutron absorption rate, will
B4C particles are added in the matrix of copper and copper alloy, by copper excellent plasticity and thermal conductivity, obtain preferable mechanical property
Energy, processing characteristics and heat conductivility, the sheet material or component for meeting different protection intensity can be prepared into, and be applied to nuclear power
The shielding application field of the dry of spentnuclear fuel, wet type storage and bearing structure.Copper-based neutron absorber material have higher intensity,
Wearability and excellent plasticity, excellent electric conductivity and thermal conductivity, there is well anti-corrosion in many media such as air, seawater
Property and relatively low thermal neutron absorption cross section.The stability of size is kept while heater in effective absorb；Due to copper and copper
Alloy has an excellent thermal conductivity, thus can be resistant to when being used in the spentnuclear fuel storage shelf with cooling system relative to
Aluminium, the higher temperature of magnesium alloy, while again because its plasticity is good and has higher modulus of elasticity, therefore extrusion rolling into
It is more prone to relatively when type and conduct engineering load assembly and safe.
Brief description of the drawings
Fig. 1, discharge plasma sintering stove principle schematic
Fig. 2, copper-based neutron absorber material cross section metallographic microstructure figure
Fig. 3, copper-based neutron absorber material vertical section ESEM displaing micro tissue topography figure
Fig. 4, copper-based neutron absorber material line scanning figure
Fig. 5, copper-based neutron absorber material bending stress strain curve
Mark project list as follows in figure：
1. servomotor, 2. seaming chucks, 3. graphite pressure heads, 4. graphite jigs, 5. thermocouples, 6. control panels, 7. controls
Button, 8. control electrical control cubicles, 9. push-down heads, 10. equipment bases, 11. vavuum pumps, 12. vacuum exhaust pipes, 13. sintering powders,
14. piece of graphite paper, 15. second graphite papers, 16. vacuum furnace bodies, 17. cooling water inlet pipes, 18. cooling water outlet pipes,
19. water temperature display screen, 20. water pump control buttons.
Embodiment：
It is further described below with reference to drawings described below；
Fig. 1 show discharge plasma sintering stove principle schematic, and each position connection will be matched correctly according to quantity, sequentially
Operation.Copper-based neutron absorber material is using made of discharge plasma sintering method, being in electric field, and thermal field and the field of force are total to
Can abolish particle surface oxide layer, scavenging material less than the temperature of material melting point sintering and avoid crystal grain from growing under same-action
Greatly, so that sintered body keeps excellent mechanical property and good particle dispersion, discharge plasma sintering stove is vertical
Structure, its structure as shown in Figure 1 is respectively 1. servomotors, 2. seaming chucks, 3. graphite pressure heads, 4. graphite jigs, 5. thermoelectricity
Idol, 6. control panels, 7. control buttons, 8. control electrical control cubicles, 9. push-down heads, 10. equipment bases, 11. vavuum pumps, 12. vacuum
Exhaust tube, 13. sintering powders, 14. piece of graphite paper, 15. second graphite papers, 16. vacuum furnace bodies, the water inlet of 17. cooling waters
Pipe, 18. cooling water outlet pipes, 19. water temperature display screens, 20. water pump control buttons.
The amount for the chemical substance that preparation uses, which has been subjected to, is pre-designed consideration within the scope of, is with gram, milliliter, millimeter
Measurement unit.
It is copper-based neutron absorber material cross section metallographic microstructure figure, as shown in the figure shown in Fig. 2：In Copper substrate uniformly
This boron carbide particles of Dispersed precipitate, the phenomenon of particle agglomeration is not occurred.
Shown in Fig. 3, scheme for copper-based neutron absorber material vertical section ESEM displaing micro tissue topography, as shown in the figure：It is copper-based
It is well combined between body, particle is uniformly distributed, and is well combined between particle and matrix, stomata, crackle etc. is not occurred and is substantially lacked
Fall into.
It is copper-based neutron absorber material line scanning figure shown in Fig. 4, the results showed that the combination interface of copper and boron carbide member
Plain transition is uniform.
It is copper-based neutron absorber material stress strain curve shown in Fig. 5, copper-based neutron absorber material bending strength is 350 ± 5
MPa。
Described above is only the better embodiment of the present invention, therefore all special according to the construction described in present patent application scope
The equivalent change or modification that sign and principle are done, is included in the range of present patent application.
Claims (2)
- A kind of 1. preparation method of copper-based neutron absorber material, it is characterised in that：Using discharge plasma sintering technique to mixing Dusty material, which applies pulse current, to be made to produce Joule heat and point discharge plasma between particle, makes locally to melt between particle Change forms metallurgical binding connection；Used chemical material is：Copper powder, boron carbide powder, absolute ethyl alcohol, hydrochloric acid, hydrofluoric acid, go from Sub- water, graphite paper, sand paper, diamond paste, its dosage unit are：Gram, milliliter, millimeter（Below）Copper powder：Cu50.066g±0.01gBoron carbide powder：B4C6.194g±0.01gAbsolute ethyl alcohol：C2H5OH200mL±5mLHydrochloric acid：HCl15mL±5mLHydrofluoric acid：HF200mL±5mLDeionized water：H2O500mL±5mLGraphite paper：CSand paper：SiC400#Diamond paste：C1.5mLPreparation process is as follows：(1) copper powder is pre-processedCopper powder is placed in progress drying and processing 1h, 100 DEG C for the treatment of temperature in vacuum drying oven；(2) boron carbide powder is pre-processed1. boron carbide powder is put into pickling processes 0.5h in hydrofluoric acid；2. boron carbide powder is taken out and rinsed repeatedly with deionized water to solution in neutrality；3. boron carbide is placed in drying and processing 2h in drying baker, 300 DEG C for the treatment of temperature；(3) claim to match somebody with somebody raw materialThe laggard luggage of powder is weighed in vacuum glove box to match somebody with somebody, and is 3 by the volume ratio of boron carbide and copper to avoid powder from aoxidizing:7 Ratio is matched, and weighs 6.194 ± 0.001g boron carbides and 50.066 ± 0.001g copper powders are fitted into ball grinder in the lump, be put into Zirconia ball seals；(4) ball mill mixingIt is 200rpm, ball milling 60min that the ball grinder assembled, which is installed to adjustment of rotational speed on ball mill,；(5) powder is loadedFour a diameter of 30mm of clip graphite paper disk, wherein two panels are previously charged into mold bottom compacting, in vacuum glove box It is interior：Ball grinder is opened, the mixed powder mixed is fitted into mould, other two panels graphite paper is finally placed in mixed powder Top, seaming chuck is pressed, the graphite jig for installing mixed powder is taken out from vacuum glove box；(6) pre-pressing dieGraphite jig equipped with mixed powder is put into pre-molding on forcing press, pressure 20MPa, time 5min, so that mixing Powder is compact formed；(7) discharge plasma sintering preparation process1. open control device and inspection apparatus；2. set heating schedule and pressurization parameter：From room temperature to 400 DEG C, time 5min；400 DEG C -600 DEG C, time 5min；600 DEG C -650 DEG C, time 2min；650 DEG C of insulation 5min；3. the graphite jig pressed in advance is put into body of heater, and is accommodated and consolidated with push-down head, in discharge plasma sintering stove, Graphite pressure head is provided with, pressure sensor is set above graphite pressure head, for detecting pressure feelings of the graphite pressure head to graphite jig Condition, it is 40MPa to the pressure of graphite jig to set discharge plasma sintering furnace pressure head；4. closing fire door, and vavuum pump is opened, make vacuum≤10-1Pa；5. opening heating schedule, while pass through situation in peephole continuous observation stove；6. heating terminates, cool down, blow-on, take out sample；(8) sample surfaces are cleanedThe graphite of sample surfaces remaining is polished off with sand paper, absolute alcohol cleaning sample is used after polishing；(9) sample is tested and analyzedTo the surface topography of obtained copper-based neutron absorber material, physical property, micro-nano mechanical property, sliding and bending deformation, in Sub- absorbent properties are tested and analyzed and characterized：Copper-based neutron absorber material consistency is measured using Archimedes's drainage；Using the copper-based neutron absorber material microscopic appearance of metallography microscope sem observation；Using scanning electron microscopic observation microstructure and fracture apperance；Copper-based neutron absorber material microcell consistency and elasticity modulus is measured using nano-hardness tester；The sliding and bending deformation of copper-based neutron absorber material is tested using universal tensile testing machine；The neutron-absorbing performance of copper-based neutron absorber material is tested using NEUTRON EMISSION instrument；Conclusion：Copper-based neutron absorber material appearance color is yellowish orange, and metallic luster is presented, and consistency is copper-based up to more than 99% Boron carbide Dispersed precipitate inside neutron absorber material, a large amount of agglomerations do not occur and are combined between particle and matrix good Good, bending strength is up to 350 ± 5MPa, and neutron-absorbing performance is up to 98%.
- A kind of 2. preparation method of copper-based neutron absorber material according to claim 1, it is characterised in that：Copper-based neutron is inhaled Receive material be using made of discharge plasma sintering method, be in electric field, under the collective effect in thermal field and the field of force with less than The temperature sintering of material melting point can abolish particle surface oxide layer, scavenging material and avoid crystal grain from growing up, so that sintering Body keeps excellent mechanical property and good particle dispersion, and discharge plasma sintering stove is vertical structure, its structure bag Include servomotor（1）, seaming chuck（2）, graphite pressure head（3）, graphite jig（4）, thermocouple（5）, control panel（6）, control press Button（7）, control electrical control cubicles（8）, push-down head（9）, equipment base（10）, vavuum pump（11）, vacuum exhaust pipe（12）, sintering powder （13）, piece of graphite paper（14）, second piece graphite paper（15）, vacuum furnace body（16）, cooling water inlet pipe（17）, cooling water goes out Water pipe（18）, water temperature display screen（19）, water pump control button（20）.
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