CN107671278B - It is single-phase to contain Mg high entropy corrosion resisting alloy powder and preparation method thereof - Google Patents
It is single-phase to contain Mg high entropy corrosion resisting alloy powder and preparation method thereof Download PDFInfo
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- CN107671278B CN107671278B CN201710934308.7A CN201710934308A CN107671278B CN 107671278 B CN107671278 B CN 107671278B CN 201710934308 A CN201710934308 A CN 201710934308A CN 107671278 B CN107671278 B CN 107671278B
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- 239000000843 powder Substances 0.000 title claims abstract description 53
- 239000001997 corrosion-resisting alloy Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000956 alloy Substances 0.000 claims abstract description 40
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 18
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 12
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical group CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000498 ball milling Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000005551 mechanical alloying Methods 0.000 claims abstract description 4
- 238000001238 wet grinding Methods 0.000 claims abstract description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 15
- 239000010935 stainless steel Substances 0.000 claims description 14
- 238000006424 Flood reaction Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims 1
- 238000005260 corrosion Methods 0.000 abstract description 45
- 230000007797 corrosion Effects 0.000 abstract description 44
- 239000000203 mixture Substances 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000010959 steel Substances 0.000 abstract 1
- 239000011777 magnesium Substances 0.000 description 57
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 28
- 239000000243 solution Substances 0.000 description 27
- 239000011780 sodium chloride Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- 229910052759 nickel Inorganic materials 0.000 description 5
- 230000010287 polarization Effects 0.000 description 5
- 239000004615 ingredient Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 229910000906 Bronze Inorganic materials 0.000 description 3
- 239000010974 bronze Substances 0.000 description 3
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B22F1/0003—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/042—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling using a particular milling fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
It is single-phase containing Mg high entropy corrosion resisting alloy dusty material and preparation method thereof that the invention discloses one kind, belongs to corrosion resisting alloy technical field.The chemical formula of the corrosion resisting alloy powder is MgxTiAlFeNiCr (x=0.6~1.4).Metal powder raw material is weighed by chemical formula, wherein Mg powder purity >=99.5%, remaining metal powder >=99%, all raw material powder particle sizes >=200 mesh.The raw material claimed is poured into stainless cylinder of steel, mechanical alloying 80~120h of wet-milling, ratio of grinding media to material 20:1, controlling agent is normal heptane, and drum's speed of rotation is 300~500rpm.After ball milling, removal normal heptane is vacuumized in glove box, is obtained by the high-entropy alloy powder of single FCC phase composition.This method preparation process is simple, efficient, yield is high, pollution-free, and obtained high-entropy alloy powder has the advantages that price is low, density is small and corrosion resistance is excellent.
Description
Technical field
The invention belongs to corrosion resisting alloy technical fields, and in particular to the single-phase entropy corrosion resisting alloy powder containing Mg high of one kind
Material system and preparation method thereof.
Background technique
High-entropy alloy is to develop very swift and violent a kind of alloy material in recent years, due to its can generate sluggish diffusion effect,
The high entropy effects such as distortion of lattice effect and " cocktail " effect, so as to cause a series of excellent characteristics, such as: high intensity and hard
Degree, excellent wear-resisting property, high temperature resistance and good corrosion resistance etc. [A.V.Kuznetsova,
D.G.Shaysultanov,N.D.Stepanov,G.A.Salishchev,O.N.Senkov,Materials Science and
Engineering A,533(2012),107.].Nearest people have developed a series of high entropy corrosion resisting alloy, such as:
AlCoCrFeNi2.1, CuCoCrNiFe, CuYZrTiHf, CoCrFeNiW, CuZrAlTiNi, AlCoCrFeTi and TiNbHfZrTi
Deng.These alloys have simple body-centered cubic (BCC) or face-centered cubic (FCC) crystal structure.Wherein, some alloys are shown
Corrosion potential more higher than 304 stainless steels, lower corrosion current speed；Such as AlCoCrFeNi2.1High-entropy alloy powder is 10%
HCl solution and corrosion potential in 3.5wt% (weight ratio) NaCl solution and corrosion electric current density be respectively -0.6242, -
1.2736V with 0.2797,0.5560A/cm2, and 304L powder of stainless steel is in 10%HCl solution and 3.5wt%NaCl solution
Corrosion potential and corrosion electric current density be respectively -0.7280, -1.3224V and 0.6300,0.58260A/cm2, illustrate ratio
Stainless steel more preferably corrosion resistance [P.P.Ding, A.Q.Mao, X.Zhang, X.Jin, B.Wang, M.Liu, Journal of
Alloys and Compounds,721(2017),609.]。
Current background technique shows that excellent high entropy corrosion resisting alloy has the feature that miscellaneous phase is fewer in (1) alloy
It is better, preferably by single simple BCC or FCC configuration phase composition；(2) the multicomponent element of alloy is transiting group metal elements,
Wherein most elements are heavy metal and yttrium；(3) the multicomponent element of alloy itself is BCC or FCC configuration.This
A little features determine under existing preparation method, and the composition range for obtaining the high-entropy alloy of phase structure is relatively narrow, preparation process
It is difficult to control.In particular, the constituent element of these high-entropy alloys be heavy metal and rare metal, increase material weight and cost,
Reduce specific strength, the specific stiffness of material.Magnesium (Mg) be the eighth-largest element of earth reserves, have density it is small, it is cheap, than strong
Spend the advantages that high；In recent years, Mg and its alloy are widely applied to the fields such as engineering device, aerospace and biologic medical.
However, the disadvantages of chemical activity of Mg is high, poor corrosion resistance limits it in the application of more wide neighborhood.Although high-entropy alloy is aobvious
Good corrosion resistance is shown；But since the crystal structure of Mg is more complex close-packed hexagonal, the original with BCC or FCC configuration
Sub- arrangement mode differs greatly；In addition, the atomic radius of Mg element and transition element differs greatly, it is former according to the formation of solid solution
Then, high-entropy alloy of the preparation containing Mg's and with simple BCC or FCC configuration is very difficult.Therefore, there is presently no develop one
Kind has the high entropy Mg containing alloy system of excellent corrosion resistance.
Summary of the invention
In order to overcome the deficiencies of the prior art, the technical problem to be solved in the present invention is to provide a kind of wide single-phase of composition range
Containing Mg high entropy corrosion resisting alloy powder systems, which can be prepared using simple mechanical alloying ball grinding method, be desirably to obtain
Alloy have more excellent corrosion resistance, be with a wide range of applications in corrosion resistant alloy powder field.
In order to solve the above technical problems, the technical scheme adopted by the invention is as follows:
(1) present invention firstly provides a kind of hexa-atomic MgxThe single-phase high corrosion-resistant conjunction of entropy of TiAlFeNiCr (x=0.6~1.4)
The material system at bronze end, composition range are as follows: it is 10.7~21.9% that Mg, which accounts for alloy atom percentage, Mg atomic ratio in alloy
After determination, the dosage such as Ti, Al, Fe, Ni and Cr element account for obtain remaining atomic percent.
(2)MgxThe preparation of the single-phase high entropy corrosion resisting alloy powder of TiAlFeNiCr (x=0.6~1.4): by described in (1)
Atomic percent weighs metal powder raw material respectively, weighs 30~50 grams altogether；Wherein the purity of Mg powder is not less than 99.5%, remaining gold
Belong to powder purity and be not less than 99%, all raw material powder particle sizes are not less than 200 mesh.It weighed raw metal powder will fall according to the ratio
Enter in stainless steel jar mill, stainless steel abrading-ball is added by ratio of grinding media to material 20:1, is subsequently poured into normal heptane (purity is greater than 99%) and floods
Ball material.Ball grinder is sealed, is put in 80~120h of mechanical alloying wet-milling on ball mill, the revolving speed of ball mill is 300~
500rpm, every 30min positive and negative rotation alternating are primary.After ball milling, ball milling cover is removed in glove box and vacuumizes 1h, is obtained
The single-phase corrosion resisting alloy powder containing Mg high entropy.The powder is applied or is sold directly as a kind of corrosion resistant material.
Compared with prior art, the present invention has following technical effect that
1, the invention is successfully prepared a kind of hexa-atomic Mg for the first timexThe single-phase high entropy corrosion resistant of TiAlFeNiCr (x=0.6~1.4)
Lose alloy powder.Its ingredient are as follows: it is 10.7~21.9% that Mg, which accounts for alloy atom percentage, after Mg atomic ratio determines in alloy, Ti,
The dosage such as Al, Fe, Ni and Cr element account for obtain remaining atomic percent；In this chemical composition ranges, high-entropy alloy ensure that
By single FCC phase composition, to realize the application in the corrosion-resistant field of the high-entropy alloy containing Mg.
2, the inexpensive Mg element of lightweight is introduced into high entropy alloy material system by the invention, and Mg element proportion is big
(atomic percent is 10.7~21.9%), making the alloy system of preparation with density, small, cheap, application range expands
The beneficial effect of (in addition to traditional high entropy corrosion resistant alloy application field, can be applied to anti-corrosion Mg based alloy and its coatings art).
3, the present invention is simple, easily-controllable, and small investment of production equipment, production process is pollution-free, is easy to industrialize big
Large-scale production；The alloy material system of preparation has excellent corrosion resistance.Compared with 304L powder of stainless steel, high entropy is closed
Corrosion potential of the bronze end in 10%HCl solution and 3.5wt%NaCl solution is higher, the corruption in 3.5wt%NaCl solution
Erosion current density substantially reduces, small 5~6 orders of magnitude of etch ratio 304L powder of stainless steel, with very excellent resistance to
The characteristic of seawater corrosion.
Detailed description of the invention
Fig. 1 is containing Mg high entropy corrosion resisting alloy x-ray diffractogram of powder；
Wherein: (a) being Mg0.6The X-ray diffractogram of TiAlFeNiCr high entropy corrosion resisting alloy powder；(b) it is
Mg1.0The X-ray diffractogram of TiAlFeNiCr high entropy corrosion resisting alloy powder；It (c) is Mg1.4The corrosion-resistant conjunction of TiAlFeNiCr high entropy
The X-ray diffractogram at bronze end.
Fig. 2 is the single-phase polarization curve containing Mg high entropy corrosion resisting alloy in 3.5wt.%NaCl solution；
Wherein: (a) being Mg0.6Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 3.5wt.%NaCl solution；
It (b) is Mg1.0Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 3.5wt.%NaCl solution；(c) it is
Mg1.4Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 3.5wt.%NaCl solution.
Fig. 3 is the single-phase polarization curve containing Mg high entropy corrosion resisting alloy in 10wt.%HCl solution；
Wherein: (a) being Mg0.6Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 10wt.%HCl solution；
It (b) is Mg1.0Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 10wt.%HCl solution；(c) it is
Mg1.4Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 10wt.%HCl solution.
Specific embodiment
In order to further appreciate that technology contents of the invention, it is made further below in conjunction with the drawings and specific embodiments
Description, but the present invention is not limited to following embodiments.
Embodiment 1
By Mg0.6The ingredient of TiAlFeNiCr weigh respectively Mg (200 mesh of granularity, purity 99.5%), Ti, Al, Fe, Ni and
Totally 40 grams of Cr powder (200 mesh of granularity, purity 99%).Weighed elemental metals powder is put into stainless steel jar mill, by ball
Stainless steel abrading-ball is added than 20:1 in material, is subsequently poured into normal heptane (purity is greater than 99%) and floods ball and material, seals ball grinder lid.
Ball grinder is placed in wet ball grinding 90h in ball mill, drum's speed of rotation 400rpm.After ball milling, taken out in glove box true
Empty 1h removes normal heptane, obtains by the Mg of single FCC configuration phase composition0.6TiAlFeNiCr high entropy corrosion resistant alloy powder is (see Fig. 1
(a): Mg0.6The X-ray diffractogram of TiAlFeNiCr high entropy corrosion resisting alloy powder).Mg0.6TiAlFeNiCr high entropy corrosion resistant alloy
Powder has good corrosion resistance: its corrosion potential and corrosion electric current density difference in 3.5wt.%NaCl solution
For -0.25V and 8.96 × 10-6A/cm2(see Fig. 2 (a): Mg0.6TiAlFeNiCr high entropy corrosion resisting alloy is in 3.5wt.%NaCl
Polarization curve in solution), corrosion potential and corrosion electric current density in 10wt.%HCl solution be respectively -0.39V and
0.57A/cm2(see Fig. 3 (a): Mg0.6Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 10wt.%HCl solution).
Embodiment 2
By Mg1.0The ingredient of TiAlFeNiCr weigh respectively Mg (200 mesh of granularity, purity 99.5%), Ti, Al, Fe, Ni and
Totally 40 grams of Cr powder (200 mesh of granularity, purity 99%).Weighed elemental metals powder is put into stainless steel jar mill, by ball
Stainless steel abrading-ball is added than 20:1 in material, is subsequently poured into normal heptane (purity is greater than 99%) and floods ball and material, seals ball grinder lid.
Ball grinder is placed in wet ball grinding 90h in ball mill, drum's speed of rotation 400rpm.After ball milling, taken out in glove box true
Empty 1h removes normal heptane, obtains by the Mg of single FCC configuration phase composition1.0TiAlFeNiCr high entropy corrosion resistant alloy powder is (see Fig. 1
(b): Mg1.0The X-ray diffractogram of TiAlFeNiCr high entropy corrosion resisting alloy powder).Mg1.0TiAlFeNiCr high entropy corrosion resistant alloy
Powder has good corrosion resistance: its corrosion potential and corrosion electric current density difference in 3.5wt.%NaCl solution
For -0.59V and 1.70 × 10-5A/cm2(see Fig. 2 (b): Mg1.0TiAlFeNiCr high entropy corrosion resisting alloy is in 3.5wt.%NaCl
Polarization curve in solution), corrosion potential and corrosion electric current density in 10wt.%HCl solution be respectively -0.44V and
0.55A/cm2(see Fig. 3 (b): Mg1.0Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 10wt.%HCl solution).
Embodiment 3
By Mg1.4The ingredient of TiAlFeNiCr weigh respectively Mg (200 mesh of granularity, purity 99.5%), Ti, Al, Fe, Ni and
Totally 40 grams of Cr powder (200 mesh of granularity, purity 99%).Weighed elemental metals powder is put into stainless steel jar mill, by ball
Stainless steel abrading-ball is added than 20:1 in material, is subsequently poured into normal heptane (purity is greater than 99%) and floods ball and material, seals ball grinder lid.
Ball grinder is placed in wet ball grinding 90h in ball mill, drum's speed of rotation 400rpm.After ball milling, taken out in glove box true
Empty 1h removes normal heptane, obtains by the Mg of single FCC configuration phase composition1.4TiAlFeNiCr high entropy corrosion resistant alloy powder is (see Fig. 1
(c): Mg1.4The X-ray diffractogram of TiAlFeNiCr high entropy corrosion resisting alloy powder).Mg1.4TiAlFeNiCr high entropy corrosion resistant alloy
Powder has good corrosion resistance: its corrosion potential and corrosion electric current density difference in 3.5wt.%NaCl solution
It is -0.80V and 1.25 × 10-5A/cm2 (see Fig. 2 (c): Mg1.4TiAlFeNiCr high entropy corrosion resisting alloy is in 3.5wt.%NaCl
Polarization curve in solution), corrosion potential and corrosion electric current density in 10wt.%HCl solution be respectively -0.45V and
0.58A/cm2 is (see Fig. 3 (c): Mg1.4Polarization curve of the TiAlFeNiCr high entropy corrosion resisting alloy in 10wt.%HCl solution).
Claims (2)
1. a kind of single-phase corrosion resisting alloy powder containing Mg high entropy of FCC, which is characterized in that the molecular formula of the alloy powder is
MgxTiAlFeNiCr, in which: x=0.6~1.4.
2. the preparation method of the single-phase entropy corrosion resisting alloy powder containing Mg high of FCC as described in claim 1, it is characterised in that including
Following steps:
(1) raw metal powder is weighed by the alloy atom percentage in alloy powder molecular formula；Wherein: the purity of Mg powder is not low
In 99.5%, remaining raw metal powder purity is not less than 99%, and all raw metal powder sizes are not less than 200 mesh；
(2) weighed raw metal powder is poured into stainless steel jar mill, stainless steel abrading-ball is added by ratio of grinding media to material 20:1, then
It pours into normal heptane and floods ball material；
(3) 80~120h of mechanical alloying wet-milling on ball mill is put in after sealing ball grinder；The revolving speed of the ball mill is 300
~500rpm, every 30min positive and negative rotation alternating are primary；
(4) after ball milling, ball milling cover is removed in glove box and is vacuumized, obtain the single-phase corrosion resisting alloy powder containing Mg high entropy
End.
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