CN112899509A - Composite material resisting molten zinc corrosion and preparation method and equipment thereof - Google Patents
Composite material resisting molten zinc corrosion and preparation method and equipment thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 99
- 239000011701 zinc Substances 0.000 title claims abstract description 83
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 79
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000005260 corrosion Methods 0.000 title claims abstract description 67
- 230000007797 corrosion Effects 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 41
- 239000000956 alloy Substances 0.000 claims abstract description 41
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 23
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 18
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 16
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- 238000012216 screening Methods 0.000 claims description 13
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- 238000012360 testing method Methods 0.000 description 15
- 239000010935 stainless steel Substances 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
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- 238000005246 galvanizing Methods 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000011195 cermet Substances 0.000 description 6
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
- C22C1/051—Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
-
- 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
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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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
- 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
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
- C22C29/14—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on borides
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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
- 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
- B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
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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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Optics & Photonics (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The embodiment of the invention discloses a molten zinc corrosion resistant composite material, a preparation method thereof and molten zinc corrosion resistant equipment, wherein the composite material comprises 68-78% of FeB, 10-20% of W and 12% of AlFeNiCoCr in percentage by mass. The AlFeNiCoCr comprises the following components in percentage by mass: 1.96-2.9 percent of aluminum powder, 24.06-48.73 percent of iron powder, 17.11-25.35 percent of nickel powder, 17.11-25.35 percent of cobalt powder and 15.09-22.34 percent of chromium powder. The composite material takes FeB as a hard phase, and takes AlFeNiCoCr high-entropy alloy and W as binding phases. According to the embodiment of the invention, FeB is used as a hard phase and has good corrosion resistance, the AlFeNiCoCr high-entropy alloy improves the brittleness of boride, the wettability between W and Zn is poor, and eutectic reaction with Zn is avoided at 450 ℃, so that the problem of poor molten zinc corrosion resistance of a binding phase in the traditional metal ceramic material is solved, and the molten zinc corrosion resistance of the material is improved.
Description
Technical Field
The invention belongs to the field of metal ceramic materials, and particularly relates to a composite material resistant to molten zinc corrosion, a preparation method of the composite material resistant to molten zinc corrosion, and equipment resistant to molten zinc corrosion.
Background
Hot dip galvanization is one of the most economical and effective methods for protecting metallic materials such as steel from atmospheric corrosion. Hot-dip galvanized products are widely used for plates, pipes, wires, belts, and hardware electric parts because of their excellent corrosion resistance, formability, and decorativeness. However, molten zinc is very corrosive to almost all single metals and most alloys. The corrosion of metal melts is always a worldwide problem which puzzles the galvanizing industry. Particularly, the equipment or parts immersed in the molten metal are subject to strong corrosion and abrasion of the molten metal, which causes frequent replacement of the equipment and reduction of production efficiency. This not only brings huge economic loss, but also causes waste of resources. At present, the materials resistant to corrosion of molten zinc mainly comprise cobalt-based superalloy materials, ceramic materials, metal ceramic materials and the like. Among them, cobalt-based superalloy materials are expensive, and ceramic materials are highly brittle and are easily deteriorated by crack formation and propagation. The metal ceramic combines good toughness of metal and excellent corrosion resistance of ceramic, and has better molten zinc corrosion resistance compared with other materials. However, the metallic binder phase tends to be the primary cause of failure of the cermet in molten zinc.
Therefore, it is an urgent problem to provide a cermet material with good corrosion resistance to molten zinc to improve the service life of hot-dip galvanizing equipment.
Disclosure of Invention
The embodiment of the invention mainly aims to provide a composite material resistant to molten zinc corrosion, a preparation method of the composite material resistant to molten zinc corrosion and equipment resistant to molten zinc corrosion, aiming at the defects and shortcomings of the prior art. In the embodiment of the invention, FeB is used as a hard phase, so that the corrosion resistance is good; w and AlFeNiCoCr are used as binding phases, so that the problem of poor molten zinc corrosion resistance of the binding phases in the traditional metal ceramic material is solved, and the molten zinc corrosion resistance of the material is improved.
In a first aspect, an embodiment of the invention discloses a preparation method of a molten zinc corrosion resistant composite material, which comprises the following steps:
mixing 1.96-2.9 wt%, 24.06-48.73 wt%, 17.11-25.35 wt% and 15.09-22.34 wt% of aluminum powder, iron powder, nickel powder, cobalt powder and chromium powder, adding 1 wt% of polyethylene glycol based on the total mass of the aluminum powder, the iron powder, the nickel powder, the cobalt powder and the chromium powder, and carrying out mechanical alloying to obtain mechanical alloying powder;
vacuum drying the mechanical alloying powder to obtain first dry powder, wherein the drying temperature is 80-110 ℃, the drying time is 8-24 h, and the vacuum degree is-0.1 MPa;
carrying out vacuum sintering, grinding and screening on the first dry powder to obtain an AlFeNiCoCr high-entropy alloy;
mixing 12% by mass of AlFeNiCoCr high-entropy alloy powder, 68-78% by mass of FeB powder and 10-20% by mass of W powder, adding polyethylene glycol which accounts for 1 wt.% of the total mass of the AlFeNiCoCr high-entropy alloy powder, the FeB powder and the W powder, and carrying out mixing and ball milling to obtain mixed powder;
vacuum drying the mixed powder to obtain second dry powder, wherein the drying temperature is 80-110 ℃, the drying time is 8-24 h, and the vacuum degree is-0.1 MPa;
performing the vacuum sintering, the grinding and the screening on the second dry powder to obtain a powdery FeB-W-AlFeNiCoCr composite material; and
and performing discharge plasma sintering on the powdery FeB-W-AlFeNiCoCr composite material to obtain a blocky FeB-W-AlFeNiCoCr composite material, wherein the sintering pressure is 50-90 MPa, the sintering temperature is 1200-1500 ℃, the heat preservation time is 4-10 min, and finally, the blocky FeB-W-AlFeNiCoCr composite material is cooled to room temperature along with a furnace.
In a second aspect, an embodiment of the present invention discloses a molten zinc corrosion resistant composite material, which includes, by mass: 68-78% of FeB, 10-20% of W and 12% of AlFeNiCoCr. The AlFeNiCoCr comprises the following components in percentage by mass: 1.96-2.9 percent of aluminum powder, 24.06-48.73 percent of iron powder, 17.11-25.35 percent of nickel powder, 17.11-25.35 percent of cobalt powder and 15.09-22.34 percent of chromium powder. The composite material takes FeB as a hard phase, and takes AlFeNiCoCr high-entropy alloy and W as binding phases.
In one embodiment of the invention, the microhardness of the composite material is 1450.7HV0.2～1664.8HV0.2。
In a third aspect, the invention discloses a preparation method of a composite material resisting molten zinc corrosion, which comprises the following steps:
mixing 1.96-2.9 wt%, 24.06-48.73 wt%, 17.11-25.35 wt% and 15.09-22.34 wt% of aluminum powder, iron powder, nickel powder, cobalt powder and chromium powder, adding polyethylene glycol, and mechanically alloying to obtain mechanically alloyed powder;
vacuum drying the mechanical alloying powder to obtain first dry powder;
carrying out vacuum sintering, grinding and screening on the first dry powder to obtain AlFeNiCoCr high-entropy alloy powder;
mixing 12% by mass of AlFeNiCoCr high-entropy alloy powder, 68-78% by mass of FeB powder and 10-20% by mass of W powder, adding polyethylene glycol, and performing mixing and ball milling to obtain mixed powder;
carrying out vacuum drying on the mixed powder to obtain second dry powder; and
and performing the vacuum sintering, the grinding and the screening on the second dry powder to obtain the powdery FeB-W-AlFeNiCoCr composite material.
In one embodiment of the invention, the mechanical alloying ball milling time is 50-60 h, the rotating speed is 300-350 r/min, and the ball-to-material ratio is 8: 1-12: 1.
In one embodiment of the invention, the ball milling time of the mixing ball milling is 1-3 h, the rotating speed is 150-250 r/min, and the ball-to-material ratio is 2: 1-5: 1.
in one embodiment of the invention, the drying temperature of the vacuum drying is 80-110 ℃, the drying time is 8-24 h, and the vacuum degree is-0.1 MPa. The vacuum degree set for vacuum sintering is 1 x 10-8MPa, wherein the temperature rising procedure of the vacuum sintering is as follows: heating from room temperature to 100 ℃ at the speed of 1-3 ℃/min, heating from 100 ℃ to 360-430 ℃ at the speed of 3-5 ℃/min, preserving heat at 360-430 ℃ for 70-100 min, heating from 360-430 ℃ to 950-1050 ℃ at the speed of 8-10 ℃/min, preserving heat at 950-1050 ℃ for 120-180 min, and finally cooling to room temperature along with a furnace.
In an embodiment of the present invention, after the vacuum sintering, the grinding, and the sieving are performed on the second dry powder to obtain a powdered FeB-W-AlFeNiCoCr composite material, the method further includes: and performing discharge plasma sintering on the powdery FeB-W-AlFeNiCoCr composite material to obtain a blocky FeB-W-AlFeNiCoCr composite material.
In one embodiment of the invention, the pressure of the spark plasma sintering is 50-90 MPa; the temperature rise procedure of the spark plasma sintering is as follows: heating from room temperature to 850-1100 ℃ at a heating rate of 160-210 ℃/min; then heating from 850-1100 ℃ to 1200-1500 ℃ at a heating rate of 25-55 ℃/min, and preserving heat for 4-10 min; and finally, cooling to room temperature along with the furnace.
In a fourth aspect, other embodiments of the invention also disclose a molten zinc corrosion resistant device, which comprises a coating prepared by spraying the powdery FeB-W-AlFeNiCoCr composite material prepared by the preparation method; or the block FeB-W-AlFeNiCoCr composite material prepared by the preparation method is prepared.
The composite material resisting molten zinc corrosion, the preparation method thereof and the equipment resisting molten zinc corrosion disclosed by the embodiment of the invention have the following advantages or beneficial effects:
examples of the invention use FeB is used as a hard phase and has good corrosion resistance; w and AlFeNiCoCr are used as binding phase, elements in the high-entropy alloy are dissolved into FeB in a solid mode, and Fe formed in the vacuum sintering process2B, and part of W and Fe in the binder phase2Reaction of B to form W2B, W and W2B has excellent molten zinc corrosion resistance, the AlFeNiCoCr high-entropy alloy improves the brittleness of boride, the wettability between W and Zn is poor, and eutectic reaction with Zn is avoided at 450 ℃, so that the problem of poor molten zinc corrosion resistance of a binding phase in the traditional metal ceramic material is solved, and the molten zinc corrosion resistance of the material is improved. In addition, the preparation method of the composite material provided by the embodiment of the invention is simple and convenient to operate, the used equipment is common, the raw materials are convenient to obtain, and the production and application are facilitated.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic flow chart of a method for preparing a molten zinc corrosion resistant composite according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the shapes of three AlFeNiCoCr high-entropy alloy powders after vacuum sintering;
FIG. 3 is a schematic diagram of the morphology of a powdered FeB-W-AlFeNiCoCr composite material after ball milling and mixing;
FIG. 4 is a powdered FeB-20 wt.% W-12 wt.% Al0.25XRD (X-ray diffraction) pattern of the FeNiCoCr composite material after ball milling and mixing;
FIG. 5 is a schematic diagram of the morphology of a powdered FeB-W-AlFeNiCoCr composite material after vacuum sintering;
FIG. 6 is a powdered FeB-20 wt.% W-12 wt.% Al0.25XRD pattern of FeNiCoCr composite material after vacuum sintering;
FIG. 7 is a schematic surface topography of a bulk FeB-W-AlFeNiCoCr composite;
FIG. 8 is a block of FeB-10 wt.% W-12 wt.% Al0.25An interface morphology graph of the FeNiCoCr composite material after being corroded in molten zinc at 450 ℃ for 10 days;
fig. 9 is a schematic structural diagram of a galvanizing system according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific implementation, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, a schematic flow chart of a method for preparing a metal ceramic composite according to an embodiment of the present invention is shown. Specifically, the preparation method of the molten zinc corrosion resistant composite material provided by the embodiment of the invention includes:
s11, mixing aluminum powder, iron powder, nickel powder, cobalt powder and chromium powder, adding polyethylene glycol, and carrying out mechanical alloying to obtain mechanical alloying powder.
S12 vacuum drying the mechanically alloyed powder to obtain a first dried powder.
S13, putting the first dry powder into a vacuum sintering furnace for vacuum sintering, grinding and screening to obtain AlFeNiCoCr high-entropy alloy powder.
S14, mixing the AlFeNiCoCr high-entropy alloy powder, the FeB powder and the W powder, adding polyethylene glycol, and performing mixing and ball milling to obtain mixed powder.
S15, vacuum drying the mixed powder to obtain a second dry powder.
S16, carrying out the vacuum sintering, the grinding and the screening on the second dry powder to obtain the powdered FeB-W-AlFeNiCoCr composite material.
Wherein, the mentioned step S11 specifically includes: mixing aluminum powder, iron powder, nickel powder, cobalt powder and chromium powder with the mass percentages of 1.96-2.9%, 24.06-48.73%, 17.11-25.35% and 15.09-22.34%, adding into a ball milling tank of a ball mill, adding polyethylene glycol which accounts for 1 wt.% of the total mass of the aluminum powder, the iron powder, the nickel powder, the cobalt powder and the chromium powder, and mixing in a ratio of 8: 1-12: adding stainless steel grinding balls according to the ball-to-material ratio (mass ratio) of 1, pouring 45-60 ml of absolute ethyl alcohol, ball-milling for 50-60 hours at the rotating speed of 300-350 r/min, and carrying out mechanical alloying to obtain mechanical alloying powder.
The mentioned step S12 specifically includes: and (3) drying the mechanical alloying powder in a vacuum environment with the drying temperature of 80-110 ℃, the drying time of 8-24 hours and the vacuum degree of-0.1 MPa to obtain first dry powder.
The mentioned step S13 specifically includes: adding the first dry powder into a vacuum sintering furnace, and vacuumizing to 1 × 10-8And (3) heating the mixture to 100 ℃ from room temperature at the speed of 1-3 ℃/min, heating the mixture to 360-430 ℃ from 100 ℃ at the speed of 3-5 ℃/min, preserving the heat at 360-430 ℃ for 70-100 min, heating the mixture to 950-1050 ℃ from 360-430 ℃ at the speed of 8-10 ℃/min, preserving the heat at 950-1050 ℃ for 120-180 min, and finally cooling the mixture to room temperature along with a furnace. And then taking out the sintered blank, grinding the blank by using a mortar, and screening by using a 60-400-mesh stainless steel sieve to obtain AlFeNiCoCr high-entropy alloy powder.
The mentioned step S14 specifically includes: mixing 12% by mass of AlFeNiCoCr high-entropy alloy powder, 68-78% by mass of FeB powder and 10-20% by mass of W powder, adding the mixture into a ball milling tank of a ball mill, adding polyethylene glycol which accounts for 1 wt.% of the total mass of the AlFeNiCoCr high-entropy alloy powder, the FeB powder and the W powder, and mixing the mixture in a ratio of 2: 1-5: 1, filling stainless steel grinding balls in a ball-to-material ratio (mass ratio) of 1, pouring 50ml of absolute ethyl alcohol, and performing ball milling for 1-3 hours at a rotating speed of 150-250 r/min to obtain uniform mixed powder.
The mentioned step S15 specifically includes: and drying the mixed powder in a vacuum environment with the drying temperature of 80-110 ℃, the drying time of 8-24 hours and the vacuum degree of-0.1 MPa to obtain second dry powder.
Mentioned stepsStep S16 specifically includes: vacuumizing the vacuum sintering furnace to 1 × 10-8And (3) heating the mixture to 100 ℃ from room temperature at the speed of 1-3 ℃/min, heating the mixture to 360-430 ℃ from 100 ℃ at the speed of 3-5 ℃/min, preserving the heat at 360-430 ℃ for 70-100 min, heating the mixture to 950-1050 ℃ from 360-430 ℃ at the speed of 8-10 ℃/min, preserving the heat at 950-1050 ℃ for 120-180 min, and finally cooling the mixture to room temperature along with a furnace. And then taking out the sintered blank, grinding the blank by using a mortar, and screening by using a 60-400-mesh stainless steel sieve to obtain the powdery FeB-W-AlFeNiCoCr composite material.
Further, the preparation method of the composite material resisting molten zinc corrosion also comprises the following steps:
s17, performing spark plasma sintering on the powdery FeB-W-AlFeNiCoCr composite material to obtain a blocky FeB-W-AlFeNiCoCr composite material.
Wherein, the mentioned step S17 specifically includes: and (3) placing the powdery FeB-W-AlFeNiCoCr composite material in a sintering furnace with the sintering pressure of 50-90 MPa, the sintering temperature of 1200-1500 ℃ and the heat preservation time of 4-10 min for spark plasma sintering, and finally cooling to room temperature along with the furnace to obtain the block FeB-W-AlFeNiCoCr composite material.
It is worth mentioning that the addition of polyethylene glycol into aluminum powder, iron powder, nickel powder, cobalt powder, chromium powder, AlFeNiCoCr high-entropy alloy powder, FeB powder and W powder is beneficial to improving the formability of the powder in vacuum sintering.
The composite material obtained by the steps takes FeB as a hard phase, and has good corrosion resistance; w and AlFeNiCoCr are used as binding phases, AlFeNiCoCr high-entropy alloy is used for improving the brittleness of boride, the wettability between W and Zn is poor, eutectic reaction does not occur between W and Zn at 450 ℃, and the problem that the corrosion resistance of the binding phases in the traditional metal ceramic material is poor is solved, so that the corrosion resistance of the material to molten zinc is improved.
In order to facilitate a better understanding of the examples of the present invention, the following 6 experiments illustrate the preparation of the composite material according to the examples of the present invention in detail.
[ TEST I ]
(X1) 50.000g of aluminum powder 1.450g, iron powder 12.030g, nickel powder 12.675g, cobalt powder 12.675g, and chromium powder 11.170g each having a purity of 99.9% and an average particle diameter of 2 μm were weighed by an electronic balance, for example, in mass percentages of 2.9%, 24.06%, 25.35%, and 22.34%, and added to a ball mill pot of a ball mill, and 0.500g of polyethylene glycol was further added thereto so as to prepare a mixture of 10: adding stainless steel balls according to the ball-to-material ratio (mass ratio) of 1, pouring 45ml of absolute ethyl alcohol, and carrying out ball milling for 50h at the rotating speed of 300r/min to obtain mechanical alloying powder.
(X2) vacuum-drying the mechanically alloyed powder obtained in the step (X1) at 100 ℃ under a vacuum of-0.1 MPa for 24 hours to obtain a first dried powder.
(X3) putting the first dry powder obtained in the step (X2) into a vacuum sintering furnace for vacuum sintering, grinding and screening to obtain Al0.25FeNiCoCr high-entropy alloy powder. Wherein, the vacuum sintering specifically comprises: vacuumizing the vacuum sintering furnace to 1 × 10-8And (2) MPa, heating from room temperature to 100 ℃ at the speed of 2 ℃/min, heating from 100 ℃ to 420 ℃ at the speed of 5 ℃/min, preserving the heat at 420 ℃ for 90min, heating from 420 ℃ to 960 ℃ at the speed of 8 ℃/min, preserving the heat at 960 ℃ for 160min, and finally cooling to room temperature along with the furnace. Then taking out the sintered blank and grinding the blank by using a stainless steel mortar, although the specific type of mortar is not limited in this embodiment, for example, the blank can be ground by using a corundum mortar and then sieved by using a 60-mesh stainless steel sieve to obtain Al0.25FeNiCoCr high-entropy alloy powder.
[ TEST II ]
The preparation method of test two was largely identical to that of test one, except that:
1) step (X1): in the following mass percentages of 2.34%, 38.79%, 20.43% and 18.01%, 60.000g of aluminum powder 1.404g, iron powder 23.274g, nickel powder 12.258g, cobalt powder 12.258g and chromium powder 10.806g, all of which have a purity of 99.9% and an average particle diameter of 2 μm, were weighed by an electronic balance, respectively, and added to a ball mill pot of a ball mill, and 0.600g of polyethylene glycol was further added so as to provide a 10: 1, adding a stainless steel grinding ball, pouring 55ml of absolute ethyl alcohol, and carrying out ball milling for 55h at the rotating speed of 300r/min to obtain mechanical alloying powder.
2) Step (X3): to obtain Al0.25Fe2NiCoCr high-entropy alloy powder.
[ TEST III ]
The preparation method of trial three was largely the same as that of trial one, except that:
1) step (X1): 1.96%, 48.73%, 17.11% and 15.09% by mass of aluminum powder having a purity of 99.9% and an average particle diameter of 2 μm, 1.176g of iron powder 29.238g, 10.266g of nickel powder, 10.266g of cobalt powder and 9.054g of chromium powder were weighed by an electronic balance, respectively, and 60.000g of the weighed materials were put into a ball mill pot of a ball mill, and 0.600g of polyethylene glycol was further added to the ball mill pot so as to prepare a mixture of 11: 1, adding a stainless steel grinding ball according to the ball-to-material ratio (mass ratio), pouring 60ml of absolute ethyl alcohol, and carrying out ball milling for 60 hours at the rotating speed of 320r/min to obtain mechanical alloying powder.
2) Step (X3): to obtain Al0.25Fe3NiCoCr high-entropy alloy powder.
The embodiment of the invention carries out morphology analysis on the AlFeNiCoCr high-entropy alloy powder obtained by the first test, the second test and the third test:
referring to FIG. 2, FIG. 2 shows the morphology of AlFeNiCoCr high-entropy alloy powder after vacuum sintering, wherein a, b and c are Al respectively0.25FeNiCoCr、Al0.25Fe2NiCoCr、Al0.25Fe3The shape of the NiCoCr high-entropy alloy powder after vacuum sintering. As shown in fig. 2, as the content of Fe element increases, the particle size of the powder after sintering gradually becomes coarse.
[ TEST FOUR ]
(Y1) weighing 7.200g of the Al0.2560g of FeNiCoCr high-entropy alloy powder, 6.000g of the W powder and 46.800g of the FeB powder are put into a ball milling tank, and 0.600g of polyethylene glycol is additionally added, so that the weight ratio of the mixture is 3: the grinding balls are filled according to the ball material ratio (mass ratio) of 1, 50ml of absolute ethyl alcohol is poured, and the ball milling is carried out for 2 hours at the rotating speed of 200r/min, so as to obtain uniform mixed powder.
(Y2) the mixed powder obtained in the step (Y1) was dried under vacuum at 90 ℃ and-0.1 MPa for 24 hours to obtain a second dried powder.
(Y3) putting the second dry powder obtained in the step (Y2) into a vacuum sintering furnace for vacuum sintering, grinding and sieving to obtain powdered FeB-10 wt.% W-12 wt.% Al0.25FeNiCoCr composite material. Wherein the vacuum sintering comprises: vacuumizing the vacuum sintering furnace to 1 × 10-8And (2) MPa, heating from room temperature to 100 ℃ at the speed of 2 ℃/min, heating from 100 ℃ to 400 ℃ at the speed of 4 ℃/min, preserving the heat at 400 ℃ for 90min, heating from 400 ℃ to 1000 ℃ at the speed of 8 ℃/min, preserving the heat at 1000 ℃ for 160min, and finally cooling to room temperature along with the furnace. Here, the grinding process in this step was the same as that in test one, and a 400 mesh stainless steel sieve was used for the sieving.
(Y4) subjecting the powdered FeB-10 wt.% W-12 wt.% Al obtained in step (Y3) to0.25FeNiCoCr composite material. Performing spark plasma sintering, wherein the pressure of the spark plasma sintering is 70 MPa; the temperature rising procedure of the spark plasma sintering is as follows: heating from room temperature to 950 ℃ at a heating rate of 160 ℃/min; then heating from 950 ℃ to 1300 ℃ at the heating rate of 40 ℃/min, and preserving heat for 7 min; finally, cooling the mixture to room temperature along with the furnace to obtain the bulk FeB with the corrosion resistance of molten zinc, namely 10 wt.% W and 12 wt.% Al0.25FeNiCoCr composite material.
[ TEST FIVE ]
The preparation method of test five is largely identical to that of test four, except that:
1) step (Y1): weighing 7.200g of the Al0.2560g of FeNiCoCr high-entropy alloy powder, 9.000g of the W powder and 43.800g of the FeB powder are put into a ball milling tank for ball milling and mixing, and finally the powdery FeB with 15 wt.% of W and 12 wt.% of Al is obtained0.25FeNiCoCr composite material.
2) Step (Y4): to obtain FeB-15 wt.% W-12 wt.% Al in bulk form0.25FeNiCoCr composite material.
[ TEST HEI ]
The preparation method of trial six was largely the same as that of trial four and trial five, except that:
1) step (Y1): weighing 7.200g of the Al0.2560g of FeNiCoCr high-entropy alloy powder, 12.000g of W powder and 40.800g of FeB powder are put into a ball milling tankBall-milling and mixing to obtain powdered FeB-20 wt.% W-12 wt.% Al0.25FeNiCoCr composite material.
2) Step (Y4): to obtain FeB-20 wt.% W-12 wt.% Al in bulk0.25FeNiCoCr composite material.
The invention is to obtain the powder FeB-W-AlFeNiCoCr composite material and the non-powder FeB-W-Al composite material from the above examples0.25Detecting and analyzing the morphology, phase and performance of the FeNiCoCr composite material:
referring to fig. 3, fig. 3 is a morphology of a powdered FeB-W-AlFeNiCoCr composite after mixing and ball milling, wherein a, b, c are powdered FeB-10 wt.% W-12 wt.% Al, respectively0.25FeNiCoCr, powdered FeB-15 wt.% W-12 wt.% Al0.25FeNiCoCr and powdered FeB-20 wt.% W-12 wt.% Al0.25The morphology of the FeNiCoCr composite material after mixing and ball milling. As shown in FIG. 3, the powdered FeB-W-AlFeNiCoCr composite material after ball milling is uniform and polygonal, which is beneficial to improving the compactness of the material, and molten zinc is difficult to permeate into the composite material through pores, thereby improving the corrosion resistance of the material.
Referring to FIG. 4, FIG. 4 is a powdered FeB-20 wt.% W-12 wt.% Al0.25XRD pattern of FeNiCoCr composite after mixing and ball milling. As shown in FIG. 4, powdered FeB-20 wt.% W-12 wt.% Al was mixed and ball milled0.25The phase of the FeNiCoCr composite material consists of FeB, W and FCC solid solution (high-entropy alloy), and the phase change does not occur in the ball milling process.
Referring to FIG. 5, FIG. 5 is a graph of powdered FeB-W-AlFeNiCoCr composite after vacuum sintering, wherein a, b, and c are powdered FeB-10 wt.% W-12 wt.% Al, respectively0.25FeNiCoCr, powdered FeB-15 wt.% W-12 wt.% Al0.25FeNiCoCr and powdered FeB-20 wt.% W-12 wt.% Al0.25Morphology of the FeNiCoCr composite after vacuum sintering. As shown in fig. 5, the powders after vacuum sintering were uniform and had a close particle size.
Referring to FIG. 6, FIG. 6 is a powdered FeB-20 wt.% W-12 wt.% Al0.25XRD pattern of FeNiCoCr composite material after vacuum sintering; as shown in FIG. 6, vacuum firingPowdered FeB-20 wt.% W-12 wt.% Al after sintering0.25The phase of the FeNiCoCr composite material consists of FeB and Fe2B. W and W2B composition, part of FeB being converted into Fe during vacuum sintering2B, high-entropy alloy elements in the binder phase are dissolved into FeB and Fe in a solid mode2B, and part of W and Fe in the binder phase2Reaction of B to form W2B. The invention adopts AlFeNiCoCr high-entropy alloy and W as binding phase, and the high-entropy alloy element is dissolved in FeB and Fe in solid solution2B to improve their brittleness, and W2B has excellent molten zinc corrosion resistance, has poor wettability between W and Zn, does not generate eutectic reaction with Zn at 450 ℃, and effectively solves the problem that the prior metal ceramic or composite material is always ineffective in molten zinc due to a binding phase.
Referring to FIG. 7, FIG. 7 shows the surface morphology of the bulk FeB-W-AlFeNiCoCr composite material, wherein a, b, and c are the bulk FeB-10 wt.% W-12 wt.% Al, respectively0.25FeNiCoCr, bulk FeB-15 wt.% W-12 wt.% Al0.25FeNiCoCr and bulk FeB-20 wt.% W-12 wt.% Al0.25Surface morphology of FeNiCoCr composite, where black represents pores.
Referring to FIG. 8, FIG. 8 is a block of FeB-10 wt.% W-12 wt.% Al0.25The interface topography of the FeNiCoCr composite material after being corroded in molten zinc at 450 ℃ for 10 days is shown in FIG. 8, and the interface topography is a bakelite powder layer, a zinc layer and a composite material layer from left to right. It can be seen that after 10 days of corrosion in molten zinc at 450 ℃, the molten zinc has not corroded the composite, indicating that the composite has excellent resistance to corrosion by molten zinc.
It is worth mentioning that the invention also applies to the bulk FeB-W-Al by using MH-5L micro Vickers hardness meter0.25The samples of the FeNiCoCr composite material were subjected to microhardness testing. Wherein the load is 200g, the loading time is 15 seconds, each sample selects 6 different positions, and the microhardness of the obtained sample is 1450.7HV0.2～1664.8HV0.2。
In addition, another embodiment of the invention provides a molten zinc corrosion resistant device, for example, comprising a cermet coating prepared by spraying the powdery FeB-W-AlFeNiCoCr composite material mentioned in the previous embodiment; or from the bulk FeB-W-AlFeNiCoCr composite material mentioned in the previous examples.
The molten zinc corrosion resistant equipment is, for example, a hot dip galvanizing furnace, but may be other equipment directly contacting molten zinc. The spraying is characterized in that high-speed airflow is generated by burning compressed air and fuel to heat the powder but not completely melt the powder, and the powder is accelerated to more than 700m/s and impacts a substrate to form a coating with extremely low oxide content and extremely high density. Namely, the molten zinc corrosion resistance equipment disclosed in this embodiment can realize molten zinc corrosion resistance by covering a cermet coating obtained by spraying a powdery FeB-W-AlFeNiCoCr composite material, or can realize molten zinc corrosion resistance by preparing a bulk FeB-W-AlFeNiCoCr composite material.
For example, as shown in fig. 9, a galvanizing system 100 resistant to molten zinc corrosion includes: a zinc bath 110, a clamping member 120 and a cermet coating 130. The mentioned zinc liquid pool 110 is used for containing zinc liquid, the mentioned clamping member 120 is used for clamping a plated part into the zinc liquid pool 110 for dip plating, and the mentioned metal ceramic coating 130 is prepared by spraying powdery FeB-W-AlFeNiCoCr composite materials, for example, by an active combustion high-speed gas spraying process, on the surfaces of the zinc liquid pool 110 and the clamping member 120. The molten zinc bath 110 and the clamping member 120 are resistant to molten zinc corrosion by being coated with a cermet coating 130, thereby improving the service life.
Of course, the aforementioned zinc bath 110 and the clamping member 120 in the galvanizing system 100 can also be designed by using the block-shaped FeB-W-AlFeNiCoCr composite material mentioned in the foregoing embodiment of the present invention as a base material, but the present embodiment is not limited thereto, and other components in the galvanizing system that directly contact with molten zinc can also be designed to resist molten zinc corrosion by using the aforementioned design, and at this time, the zinc bath 110 and the clamping member 120 no longer need to be sprayed with a coating, so as to have excellent molten zinc corrosion resistance.
In summary, the embodiments of the present inventionThe embodiment of the invention takes FeB as a hard phase and has good corrosion resistance; w and AlFeNiCoCr are used as binding phase, elements in the high-entropy alloy are dissolved into FeB in a solid mode, and Fe formed in the vacuum sintering process2B, and part of W and Fe in the binder phase2Reaction of B to form W2B, W and W2B has excellent molten zinc corrosion resistance, the AlFeNiCoCr high-entropy alloy improves the brittleness of boride, the wettability between W and Zn is poor, and eutectic reaction with Zn is avoided at 450 ℃, so that the problem of poor molten zinc corrosion resistance of a binding phase in the traditional metal ceramic material is solved, and the molten zinc corrosion resistance of the material is improved. In addition, the preparation method of the composite material provided by the embodiment of the invention is simple and convenient to operate, the used equipment is common, the raw materials are convenient to obtain, and the production and application are facilitated.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of a composite material resisting molten zinc corrosion is characterized by comprising the following steps:
mixing 1.96-2.9 wt%, 24.06-48.73 wt%, 17.11-25.35 wt% and 15.09-22.34 wt% of aluminum powder, iron powder, nickel powder, cobalt powder and chromium powder, adding 1 wt% of polyethylene glycol based on the total mass of the aluminum powder, the iron powder, the nickel powder, the cobalt powder and the chromium powder, and carrying out mechanical alloying to obtain mechanical alloying powder;
vacuum drying the mechanical alloying powder to obtain first dry powder, wherein the drying temperature is 80-110 ℃, the drying time is 8-24 h, and the vacuum degree is-0.1 MPa;
carrying out vacuum sintering, grinding and screening on the first dry powder to obtain an AlFeNiCoCr high-entropy alloy;
mixing 12% by mass of AlFeNiCoCr high-entropy alloy powder, 68-78% by mass of FeB powder and 10-20% by mass of W powder, adding polyethylene glycol which accounts for 1 wt.% of the total mass of the AlFeNiCoCr high-entropy alloy powder, the FeB powder and the W powder, and carrying out mixing and ball milling to obtain mixed powder;
vacuum drying the mixed powder to obtain second dry powder, wherein the drying temperature is 80-110 ℃, the drying time is 8-24 h, and the vacuum degree is-0.1 MPa;
performing the vacuum sintering, the grinding and the screening on the second dry powder to obtain a powdery FeB-W-AlFeNiCoCr composite material; and
and performing discharge plasma sintering on the powdery FeB-W-AlFeNiCoCr composite material to obtain a blocky FeB-W-AlFeNiCoCr composite material, wherein the sintering pressure is 50-90 MPa, the sintering temperature is 1200-1500 ℃, the heat preservation time is 4-10 min, and finally, the blocky FeB-W-AlFeNiCoCr composite material is cooled to room temperature along with a furnace.
2. A composite material resistant to corrosion by molten zinc, characterized by comprising, in mass percent: 68-78% of FeB, 10-20% of W and 12% of AlFeNiCoCr;
the AlFeNiCoCr comprises the following components in percentage by mass: 1.96-2.9 percent of aluminum powder, 24.06-48.73 percent of iron powder, 17.11-25.35 percent of nickel powder, 17.11-25.35 percent of cobalt powder and 15.09-22.34 percent of chromium powder;
the composite material takes FeB as a hard phase, and takes AlFeNiCoCr high-entropy alloy and W as binding phases.
3. The molten zinc corrosion resistant composite material of claim 2, wherein the microhardness of the composite material is 1450.7HV0.2～1664.8HV0.2。
4. A preparation method of a composite material resisting molten zinc corrosion is characterized by comprising the following steps:
mixing 1.96-2.9 wt%, 24.06-48.73 wt%, 17.11-25.35 wt% and 15.09-22.34 wt% of aluminum powder, iron powder, nickel powder, cobalt powder and chromium powder, adding polyethylene glycol, and mechanically alloying to obtain mechanically alloyed powder;
vacuum drying the mechanical alloying powder to obtain first dry powder;
carrying out vacuum sintering, grinding and screening on the first dry powder to obtain AlFeNiCoCr high-entropy alloy powder;
mixing 12% by mass of AlFeNiCoCr high-entropy alloy powder, 68-78% by mass of FeB powder and 10-20% by mass of W powder, adding polyethylene glycol, and performing mixing and ball milling to obtain mixed powder;
carrying out vacuum drying on the mixed powder to obtain second dry powder; and
and performing the vacuum sintering, the grinding and the screening on the second dry powder to obtain the powdery FeB-W-AlFeNiCoCr composite material.
5. The preparation method of the molten zinc corrosion resistant composite material according to claim 4, wherein the mechanical alloying ball milling time is 50-60 h, the rotating speed is 300-350 r/min, and the ball-to-material ratio is 8: 1-12: 1.
6. the preparation method of the molten zinc corrosion resistant composite material according to claim 4, wherein the ball milling time of the mixing ball milling is 1-3 h, the rotating speed is 150-250 r/min, and the ball-to-material ratio is 2: 1-5: 1.
7. the method for preparing the molten zinc corrosion resistant composite material according to claim 4, wherein the drying temperature of the vacuum drying is 80-110 ℃, the drying time is 8-24 h, and the vacuum degree is-0.1 MPa;
the vacuum degree set for vacuum sintering is 1 x 10-8MPa, wherein said vacuum sinteringThe temperature raising program is as follows: heating from room temperature to 100 ℃ at the speed of 1-3 ℃/min, heating from 100 ℃ to 360-430 ℃ at the speed of 3-5 ℃/min, preserving heat at 360-430 ℃ for 70-100 min, heating from 360-430 ℃ to 950-1050 ℃ at the speed of 8-10 ℃/min, preserving heat at 950-1050 ℃ for 120-180 min, and finally cooling to room temperature along with a furnace.
8. The method of claim 4, further comprising, after the vacuum sintering, the grinding, and the sieving of the second dry powder to obtain a powdered FeB-W-AlFeNiCoCr composite material:
and performing discharge plasma sintering on the powdery FeB-W-AlFeNiCoCr composite material to obtain a blocky FeB-W-AlFeNiCoCr composite material.
9. The method for preparing the molten zinc corrosion-resistant composite material according to claim 8, wherein the pressure of the spark plasma sintering is 50-90 MPa; the temperature rise procedure of the spark plasma sintering is as follows: heating from room temperature to 850-1100 ℃ at a heating rate of 160-210 ℃/min; then heating from 850-1100 ℃ to 1200-1500 ℃ at a heating rate of 25-55 ℃/min, and preserving heat for 4-10 min; and finally, cooling to room temperature along with the furnace.
10. A molten zinc corrosion resistant device, which is characterized by comprising a coating prepared by spraying the powdery FeB-W-AlFeNiCoCr composite material prepared by the preparation method of any one of claims 4 to 7; or
The bulk FeB-W-AlFeNiCoCr composite material prepared by the preparation method of claim 8 or 9.
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