CN105950915B - A kind of nanometer grade powder Mg2The preparation method of Ni compounds - Google Patents
A kind of nanometer grade powder Mg2The preparation method of Ni compounds Download PDFInfo
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- CN105950915B CN105950915B CN201610317838.2A CN201610317838A CN105950915B CN 105950915 B CN105950915 B CN 105950915B CN 201610317838 A CN201610317838 A CN 201610317838A CN 105950915 B CN105950915 B CN 105950915B
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- 239000000843 powder Substances 0.000 title claims abstract description 25
- 150000001875 compounds Chemical class 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000011777 magnesium Substances 0.000 claims abstract description 47
- 229910000990 Ni alloy Inorganic materials 0.000 claims abstract description 29
- ATTFYOXEMHAYAX-UHFFFAOYSA-N magnesium nickel Chemical compound [Mg].[Ni] ATTFYOXEMHAYAX-UHFFFAOYSA-N 0.000 claims abstract description 28
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910019758 Mg2Ni Inorganic materials 0.000 claims abstract description 13
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- 238000005260 corrosion Methods 0.000 claims abstract description 9
- 230000007797 corrosion Effects 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 5
- 239000000956 alloy Substances 0.000 claims description 21
- 229910045601 alloy Inorganic materials 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- 239000011159 matrix material Substances 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000000265 homogenisation Methods 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 5
- 238000011282 treatment Methods 0.000 claims description 5
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 3
- 239000013618 particulate matter Substances 0.000 claims description 3
- 238000007670 refining Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- PRORZGWHZXZQMV-UHFFFAOYSA-N azane;nitric acid Chemical compound N.O[N+]([O-])=O PRORZGWHZXZQMV-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000001125 extrusion Methods 0.000 claims 1
- 239000011888 foil Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 238000003860 storage Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910002804 graphite Inorganic materials 0.000 abstract description 2
- 239000010439 graphite Substances 0.000 abstract description 2
- 238000011175 product filtration Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 6
- 238000004626 scanning electron microscopy Methods 0.000 description 6
- 230000005496 eutectics Effects 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 2
- 229910017973 MgNi2 Inorganic materials 0.000 description 2
- 229910000905 alloy phase Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 238000005204 segregation Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229910000521 B alloy Inorganic materials 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000005549 size reduction Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C23/00—Alloys based on magnesium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C3/00—Removing material from alloys to produce alloys of different constitution separation of the constituents of alloys
- C22C3/005—Separation of the constituents of alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/06—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of magnesium or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/22—Acidic compositions for etching magnesium or alloys thereof
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- Chemical & Material Sciences (AREA)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
A kind of nanometer grade powder Mg2The preparation method of Ni compounds, belongs to technical field of material, and magnesium-nickel alloy is processed using severe plastic deformation technology, its microscopic structure is fully refined, Mg therein2Ni phase sizes are reduced to nanoscale, then erode the magnesium of body portion, by corrosion product filtration drying, so as to obtain the nanometer grade powder Mg of particle size uniformity2Ni.Present invention process is simple and reliable, and cost is low, obtained nanometer grade powder Mg2Ni has the size suitable with spheroidal graphite method, due to living through severe plastic deformation, Mg in preparation process2Retain larger dislocation density and distortion of lattice in Ni crystal, this is greatly improved to its hydrogen storage property tool.
Description
Technical field
The invention belongs to technical field of material, more particularly to a kind of nanometer grade powder Mg2The preparation of Ni compounds
Method.
Background technology
Hydrogen Energy is a kind of energy of clean and effective, is also the important development direction of future source of energy, and wherein novel high-performance is stored up
Hydrogen material is the key that Hydrogen Technology makes a breakthrough.Mg2Ni compounds are that there is one kind higher hydrogen storage ability and good suction to put hydrogen
Dynamic (dynamical) material.Mg2Ni powder body materials are prepared generally by rapid melting freezing method, i.e., first by magnesium and Ni-B alloy into alloy
Compound ingot casting, then the method centrifuged by heating fusing are prepared into powder body material, then again using ball milling and machinery conjunction
The nanometer grade powder hydrogen storage material that aurification method is prepared, its preparation technology is complicated and the cycle is long, and atmosphere is needed in mechanical milling process
Protection, therefore material preparation cost is higher.
The content of the invention
The present invention seeks to propose a kind of to prepare the low nanometer grade powder Mg of cost2The preparation method of Ni compounds.
The present invention comprises the following steps：
1）Nickel is added in the magnesium after fusing, magnesium-nickel alloy ingot casting is cast into after agitated, refining treatment；
2）Magnesium-nickel alloy ingot casting is subjected to homogenization heat treatment；
3）Equal-channel Angular Pressing is carried out to the magnesium-nickel alloy ingot casting after heat treatment；
4）Alloy after Equal-channel Angular Pressing is handled is processed by multi pass drawing into magnesium-nickel alloy silk or rolling
Into magnesium-nickel alloy paper tinsel；
5）Magnesium-nickel alloy silk or magnesium-nickel alloy paper tinsel are soaked in acid solution, the magnesium of matrix eroded, then by corruption
Etching off obtains solid particulate matter except method of the product to centrifuge or filter of matrix magnesium, separation, through dry nanoscale
Mg2Ni compounds.
The present invention is processed using severe plastic deformation technology to magnesium-nickel alloy, obtains its microscopic structure fully thin
Change, Mg therein2Ni phase sizes are reduced to nanoscale, then erode the magnesium of body portion, by corrosion product filtration drying,
So as to obtain the nanometer grade powder Mg of particle size uniformity2Ni。
Present invention process is simple and reliable, and cost is low, and obtained nanometer grade powder Mg2Ni has suitable with spheroidal graphite method
Size, due to living through severe plastic deformation, Mg in preparation process2Retain larger dislocation density and lattice in Ni crystal
Distortion, this is greatly improved to its hydrogen storage property tool.
Further, Mg2Nickel content weight percent hundred is about 54.7% in Ni compounds, if directly according to this ratio
Single Mg can't be directly formed in melting, alloy2Ni compounds, but form Mg2Ni、MgNi2With tri- kinds of phases of Mg, wherein
MgNi2The not effect of hydrogen storage, and nickel content it is too high can cause alloy fragility increase, plastic deformation ability decline；Nickel contains
Mg in the too low then alloy of amount2Ni phases content is very little, it is impossible to prepare enough Mg2Ni powders.It is therefore preferred that institute of the present invention
State in alloy cast ingot, nickel accounts for the 5.0~40.0% of alloy cast ingot gross mass.
The temperature conditionss of the homogenization heat treatment are 500 DEG C.Component segregation can be preferably eliminated under the temperature conditionss.
During the casting solidification of alloy, thick eutectic structure is easily formed on matrix crystal boundary, the modeling of thick eutectic in material
Property deformation process in easily ftracture, cause material processing characteristics decline.Homogenization Treatments can make the solute in eutectic former
Son is migrated by spreading, and is eutectic size reduction.
Deformation temperature conditionss are 200 DEG C~250 DEG C during the Equal-channel Angular Pressing processing, are processed using multi-pass.It is many
The Equal-channel Angular Pressing processing of passage, the thinning effect that microscopic structure is processed at a lower temperature is preferable.By many
Passage Equal-channel Angular Pressing refinement microstructure, controls the size of alloy phase.Mg2The average grain diameter of Ni phases is minimum to be reduced
To about 100 nanometers, and follow-up drawing or rolling mill practice can further reduce Mg2The size of Ni phases, and finally give
Mg2The size of Ni powders remains in this size.
The diameter of the magnesium-nickel alloy silk is in below 0.5mm.Magnesium-nickel alloy silk diameter is smaller, and the total deformation of material is got over
Greatly, Mg in alloy2Ni size is relatively also smaller, is distributed about uniform.And the ratio surface of the magnesium-nickel alloy silk smaller material of diameter
Product is bigger, is easier to fall matrix corrosion in corrosion process, obtains Mg2Ni compound powders.
Similarly, the thickness of the magnesium-nickel alloy paper tinsel is in below 0.5mm.
The acid solution is the aqueous solution of dust technology, watery hydrochloric acid or acetic acid,diluted.Corrosion when, magnesium-nickel alloy silk or
Hydrogen ion during magnesium matrix in person's paper tinsel is easy while being corroded also is reduced, and solution pH value rises, anti-using dilute acid soln
Answer speed ratio shallower, can reach that only corrosion magnesium matrix retains Mg2The effect of Ni compounds.
The acid solution be dense ammonium chloride, or concentrated nitric acid ammonium the aqueous solution.Ammonium chloride and ammonium nitrate are all strong acid weak bases
Ammonium ion is hydrolyzed in salt, its aqueous solution, solution in acidity, even but concentrated solution it is acid also weaker, in magnesium-nickel alloy
Magnesium matrix corrosion rate it is very fast, and to Mg2The corrosive effect of Ni compounds is weaker, so easily by Mg2Ni compounds are extracted
Come.
Brief description of the drawings
Fig. 1 is the Mg-10Ni alloy scanning electron microscopies of as cast condition（2000 times of amplification）.
Fig. 2 is the low power scanning electron microscopy of the Mg-10Ni alloys for the silk material for being drawn into 0.3 millimeter of diameter（Amplification
2000 times）Figure.
Fig. 3 is the high power scanning electron microscopy of the Mg-10Ni alloys for the silk material for being drawn into 0.3 millimeter of diameter（Amplification
10000 times）Figure.
Embodiment
First, preparation process is as follows：
1st, nickel is gradually added into after magnesium is melted, alloy cast ingot is cast into by stirring, refining treatment etc..
The chemical composition mass percent for the magnesium-nickel alloy that this technology is directed to is：Nickel 5.0-40.0%, remaining is magnesium and can not
The impurity avoided.
Following table is the raw material proportioning table of each example（Unit is：kg）
The 2nd, each alloy cast ingot is carried out to less than 500 DEG C of Homogenization Treatments respectively, component segregation is eliminated.
3rd, each alloy cast ingot is subjected to Equal-channel Angular Pressing（equal-channel angular pressing,
ECAP）, multi-pass processing can be repeated, every time deformation temperature is between 200 DEG C to 250 DEG C, in relatively low temperature
The thinning effect of lower processing microscopic structure is preferable.
4th, the magnesium-nickel alloy after Equal-channel Angular Pressing is handled is by the way that multi pass drawing is into magnesium-nickel alloy silk or rolls
It is processed into magnesium-nickel alloy paper tinsel, the thickness of silk material diameter and paper tinsel is in below 0.5mm.
5th, by magnesium-nickel alloy silk or paper tinsel immersion in an acidic solution, the magnesium of matrix is eroded, then by the production of corrosion
Thing is centrifuged or the method for filtering separates solid particulate matter, and drying can obtain nano level Mg2Ni powder.
Above acid solution can be the acid such as dust technology, watery hydrochloric acid, acetic acid the aqueous solution or dense ammonium chloride,
The aqueous solution of ammonium nitrate.
2nd, this technology has two advantages：One is to reach refinement microstructure by multi-pass Equal-channel Angular Pressing, control
The effect of the size of alloy phase.Mg2The average grain diameter of Ni phases is minimum can be reduced to about 100 nanometers, and follow-up drawing or
Rolling mill practice can further reduce Mg2The size of Ni phases, and the Mg finally given2It is big that the size of Ni powders remains in this
It is small.Two be to prepare relative inexpensiveness, and manufacturing cycle is shorter, can meet the production requirement of mass.
From the Mg-10Ni alloy scanning electron microscopies of Fig. 1 as cast condition：White portion is Mg2Ni phases, in latticed
Distribution, size is very thick.
From the low power scanning electron microscopy of the Mg-10Ni alloys of Fig. 2 silk material for being drawn into 0.3 millimeter of diameter：
The Mg of white2Ni phase sizes are tiny, and distribute very evenly.
From the high power scanning electron microscopy of the Mg-10Ni alloys of Fig. 3 silk material for being drawn into 0.3 millimeter of diameter：
Mg2Ni phase particle fine uniforms, average diameter is in 500 rans.
Claims (8)
1. a kind of nanometer grade powder Mg2The preparation method of Ni compounds, it is characterised in that comprise the following steps：
1）Nickel is added in the magnesium after fusing, magnesium-nickel alloy ingot casting is cast into after agitated, refining treatment；
2）Magnesium-nickel alloy ingot casting is subjected to homogenization heat treatment；
3）Equal-channel Angular Pressing is carried out to the magnesium-nickel alloy ingot casting after heat treatment；
4）Alloy after Equal-channel Angular Pressing is handled is processed into magnesium by multi pass drawing into magnesium-nickel alloy silk or rolling
Nickel alloy foil；
5）Magnesium-nickel alloy silk or magnesium-nickel alloy paper tinsel are soaked in acid solution, the magnesium of matrix is eroded, then corrosion is gone
Method except the product of matrix magnesium to centrifuge or filter, separation obtains solid particulate matter, through dry nanoscale Mg2Ni
Compound.
2. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：The alloy cast ingot
In, nickel accounts for the 5.0~40.0% of alloy cast ingot gross mass.
3. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：The homogenization heat
The temperature conditionss of processing are 500 DEG C.
4. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：It is described to wait passage to turn
It is 200 DEG C~250 DEG C that temperature conditionss are deformed during the extrusion process of angle, is processed using multi-pass.
5. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：The magnesium-nickel alloy
The diameter of silk is in below 0.5mm.
6. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：The magnesium-nickel alloy
The thickness of paper tinsel is in below 0.5mm.
7. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：The acid solution
For the aqueous solution of dust technology, watery hydrochloric acid or acetic acid,diluted.
8. nanometer grade powder Mg according to claim 12The preparation method of Ni compounds, it is characterised in that：The acid solution
For the aqueous solution of dense ammonium chloride, or concentrated nitric acid ammonium.
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| CN110129640B (en) * | 2019-06-28 | 2020-05-05 | 江西理工大学 | 7000 series aluminum alloy wire for additive manufacturing and preparation method thereof |
| CN110184492B (en) * | 2019-06-28 | 2020-07-03 | 江西理工大学 | TiB2Particle reinforced aluminum-based composite material and preparation method thereof |
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| JP4851294B2 (en) * | 2006-10-12 | 2012-01-11 | 古河電気工業株式会社 | Method for producing hydrogen storage material and hybrid powder |
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