CN113957327A - Preparation method of zinc liquid corrosion resistant FeCrBAL alloy - Google Patents
Preparation method of zinc liquid corrosion resistant FeCrBAL alloy Download PDFInfo
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- CN113957327A CN113957327A CN202111210778.1A CN202111210778A CN113957327A CN 113957327 A CN113957327 A CN 113957327A CN 202111210778 A CN202111210778 A CN 202111210778A CN 113957327 A CN113957327 A CN 113957327A
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- alloy
- zinc liquid
- fecrbal
- iron
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/04—Making ferrous alloys by melting
- C22C33/06—Making ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D6/00—Heat treatment of ferrous alloys
- C21D6/002—Heat treatment of ferrous alloys containing Cr
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/06—Ferrous alloys, e.g. steel alloys containing aluminium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C38/00—Ferrous alloys, e.g. steel alloys
- C22C38/18—Ferrous alloys, e.g. steel alloys containing chromium
- C22C38/32—Ferrous alloys, e.g. steel alloys containing chromium with boron
Abstract
The invention belongs to the field of iron-based alloy corrosion prevention for a zinc pot, and particularly relates to a preparation method of a zinc liquid corrosion resistant FeCrBAL alloy. The method comprises the following steps: repeatedly smelting the chromium, the aluminum, the iron and the Fe-B intermediate alloy serving as raw materials by using a vacuum smelting furnace for 3-5 times, and carrying out vacuum annealing to obtain an iron-based alloy; then, carrying out surface treatment on the iron-based alloy by using a high-vacuum tube furnace through a pre-oxidation method, wherein the pre-oxidation temperature is 800-850 ℃, and the oxygen pressure is 10‑25atm～10‑20atm and the oxidation time is 15-25 h. The zinc liquid corrosion resistance prepared by the method of the inventionThe etched FeCrBAL alloy surface forms a corrosion resistant oxide layer in which Al is formed by alpha-Fe phase2O3The oxide layer has very good zinc corrosion resistance, Fe2The corrosion resistance of the B phase is further improved, and the overall zinc liquid corrosion resistance of the alloy is greatly improved.
Description
Technical Field
The invention belongs to the field of iron-based alloy corrosion prevention for a zinc pot, and particularly relates to a preparation method of a zinc liquid corrosion resistant FeCrBAL alloy.
Background
Steel, which is the material used in the largest amount among all metals, has a very important position in promoting the development of various countries. However, the corrosion damage of steel materials causes huge economic loss, and the development of steel is severely limited to a certain extent. The hot dip galvanizing process is a method capable of well protecting steel materials from corrosion, zinc on the surface layer of a matrix is corroded preferentially so as to delay the corrosion of the matrix, however, in the hot dip galvanizing production process, because the zinc pot and internal components (a heater, a three-roller six-arm and the like) are corroded in a high-temperature molten liquid environment all the time, the zinc pot and the internal components (the heater, the three-roller six-arm and the like) need to be stopped and replaced regularly, and huge financial and manpower losses are caused to enterprises. In order to solve this problem, many researchers have paid great efforts, mainly from the viewpoint of improving the corrosion resistance of the entire material, and among them, since Fe — B alloys have been widely studied for their high strength and excellent corrosion resistance, the corrosion resistance of the alloys is optimized mainly by alloying methods, and Cr, Al, Ni, and other elements are generally added to the alloys, but the expected effects are not achieved.
Disclosure of Invention
The invention aims to better improve the zinc liquid corrosion resistance of the FeCrBAl alloy, and provides a preparation method of the FeCrBAl alloy with zinc liquid corrosion resistance. The invention selects Fe-20Cr-5B-3Al alloy with better overall performance and corrosion resistance to carry out preoxidation treatment, and applies preoxidation to the corrosion of the alloy, so the invention has important significance on how to improve the corrosion resistance of the iron-based material for the zinc pot.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a FeCrBAL alloy resistant to zinc liquid corrosion comprises the following steps: and repeatedly smelting the chromium, the aluminum, the iron and the Fe-B intermediate alloy as raw materials by using a vacuum smelting furnace for 3-5 times (preferably 5 times), and then carrying out vacuum annealing to obtain the iron-based alloy. The components of the iron-based alloy can be more uniform through annealing, and the annealing conditions are preferably as follows: the temperature is 1000 ℃, and the annealing time is 72 h.
The boron element is introduced in the Fe-B intermediate alloy mode, so that the burning loss of the boron element at high temperature can be reduced, and preferably, the mass percentage of the boron element in the Fe-B intermediate alloy is 10-25% (more preferably 20%).
Then, carrying out surface treatment on the iron-based alloy by using a high-vacuum tube furnace through a pre-oxidation method, wherein the pre-oxidation temperature is 800-850 ℃, and the oxygen pressure is 10-25atm～10-20atm (the temperature is too low/the oxygen pressure is too low to achieve the purpose of film formation, and if the temperature is beyond the range, the film is explosively grown to form loose and porous iron-rich oxide), and the oxidation time is 15-25 h.
Preferably, the iron-based alloy comprises 20 percent of chromium, 5 percent of boron, 3 percent of aluminum and the balance of iron by weight percent, and the Fe-20Cr-5B-3Al alloy can be obtained under the mixture ratio, and mainly comprises Fe2B and two phases of alpha-Fe, Fe2B has good corrosion resistance, and the zinc liquid can bypass Fe in the corrosion process2Phase B preferentially corrodes the alpha-Fe phase. Al is generated on the alpha-Fe phase after the surface treatment by pre-oxidation2O3Layer, having barrier effect against zinc bath, and Fe2The phase B still keeps higher corrosion resistance, thereby improving the corrosion resistance of the whole alloy. The invention improves the corrosion resistance of the iron-based alloy, and the Fe-20Cr-5B-3Al alloy is smelted by optimizing the alloy components and then is heated to 850 ℃ and 10 DEG C-20.5Pre-oxidation surface treatment is carried out under the atm condition, micron-scale oxidation films are generated on the surface of the alloy, and the micron-scale oxidation films are not generatedThe mechanical properties of the alloy are destroyed.
Preferably, the pre-oxidation temperature is 850 ℃ and the oxygen pressure is 10-20.5atm and an oxidation time of 20 h.
Compared with the prior art, the invention has the following technical effects:
the surface of the FeCrBAL alloy which is resistant to the corrosion of the zinc liquid and prepared by the method of the invention forms an oxide layer with strong corrosion resistance, and the method specifically comprises the following steps: iron-based alloys including Fe2B and alpha-Fe phase, in which Fe2The phase B has high corrosion resistance, and the corrosion resistance of alpha-Fe is poor; corrosion-resistant Al is generated on the alpha-Fe phase with poor corrosion resistance by pre-oxidation2O3Oxide layer of Fe having good corrosion resistance2A Cr-B mixed oxide layer is formed on the B phase. The advantage of this is Al formed by alpha-Fe phase2O3The oxide layer has very good zinc corrosion resistance, Fe2The corrosion resistance of the B phase is further improved, and the overall zinc liquid corrosion resistance of the alloy is greatly improved.
Drawings
The accompanying drawings, which are described herein, are included to provide a further explanation of the invention and are incorporated in and constitute a part of this application, and the description of the invention as illustrated is intended to explain the invention and is not to be construed as limiting the invention.
FIG. 1: schematic representation of the high vacuum tube furnace used for pre-oxidation in example 2;
FIG. 2: surface texture topography after annealing of the alloy of example 1;
FIG. 3: example 1 SEM image of cross-section of non-pre-oxidized alloy after etching in 600 ℃ zinc bath for 48 h;
FIG. 4: in the embodiment, SEM pictures of cross sections of the alloy after being pre-oxidized and being corroded for 48 hours in a zinc liquid at 600 ℃, wherein (a), (b) and (c) are corrosion cross sections after being oxidized for 15 hours, 20 hours and 25 hours respectively;
FIG. 5: (a) SEM pictures of alloy sections after 5h and 10h of oxidation respectively, (c) a corrosion section of a sample after 10h of oxidation, and (d) a surface picture after 30h of oxidation;
FIG. 6: 900 ℃ and 10-16.8Pre-oxidizing the alloy for 5h under the atm condition and then combiningCross-sectional view of gold.
Detailed Description
The present invention is not limited to the following embodiments, and those skilled in the art can implement the present invention in other embodiments according to the disclosure of the present invention, or make simple changes or modifications on the design structure and idea of the present invention, and fall into the protection scope of the present invention. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The invention is described in more detail below with reference to the following examples:
in the following examples, the materials used in this patent are provided by Beijing Liyuanxinxin metallic materials science and technology Co., Ltd, wherein the Fe-B alloy is irregular block with specification of 10mm × 10mm, and the rest materials are all specification
But this is not a limitation on the scope of the present application.
Example 1
(1) The alloy is prepared by a weight percentage method, the content of the chromium is 20 percent, the boron is 5 percent, the aluminum is 3 percent, and the balance is iron, wherein the boron element is easy to burn at high temperature, and the boron element is added by a method of Fe-B (the boron content is 20 percent) intermediate alloy. And repeatedly smelting the proportioned material for 5 times by using a vacuum smelting furnace to ensure the uniformity of alloy components.
(2) And (2) placing the alloy smelted in the step (1) in a vacuum annealing furnace at 1000 ℃ for annealing treatment for 72 hours to make the components uniform.
(3) Cutting the alloy treated in the step (2) into rectangular blocks with the size of 30 multiplied by 20 multiplied by 10mm by a wire cutting machine, then grinding and polishing the alloy by 400-mesh, 1000-mesh and 2000-mesh sandpaper, and placing the alloy in a vacuum drying oven with the temperature of 50 ℃ for later use.
(4) 1kg of zinc ingot (with the purity of 99.9%) is placed in a resistance furnace at 600 ℃, after the zinc ingot is melted, the alloy in the step (3) is placed in the resistance furnace, and a corrosion experiment is carried out for 48 hours.
Example 2
(1) The alloy is prepared by a weight percentage method, the content of the chromium is 20 percent, the boron is 5 percent, the aluminum is 3 percent, and the balance is iron, wherein the boron element is easy to burn at high temperature, and the boron element is added by a method of Fe-B (the boron content is 20 percent) intermediate alloy. And repeatedly smelting the proportioned material for 5 times by using a vacuum smelting furnace to ensure the uniformity of alloy components.
(2) And (2) placing the alloy smelted in the step (1) in a vacuum annealing furnace at 1000 ℃ for annealing treatment for 72 hours to make the components uniform.
(3) Cutting the alloy treated in the step (2) into rectangular blocks with the size of 30 multiplied by 20 multiplied by 10mm by a wire cutting machine, then carrying out grinding and polishing treatment on the alloy by 400-mesh, 1000-mesh and 2000-mesh sandpaper, and then placing the alloy in a vacuum drying oven with the temperature of 50 ℃ for standby.
(4) Putting the alloy sample treated in the step (3) into a high vacuum tube furnace for vacuumizing treatment, and then carrying out preoxidation surface treatment on the alloy, wherein the preoxidation temperature is 850 ℃, and the oxygen pressure is 10-20.5atm, and the oxidation time is 15h, 20h and 25h respectively.
(5) 1kg of zinc ingot (with the purity of 99.9%) is placed in a resistance furnace at 600 ℃, after melting, the alloy after pre-oxidation treatment is placed in the resistance furnace, and a corrosion experiment is carried out for 48 hours.
Effects of the embodiment
The surface structure of the alloy without the pre-oxidation surface treatment is shown in FIG. 2, and it can be seen that the alloy is mainly composed of Fe2B and alpha-Fe; the morphology of the alloy surface after the pre-oxidation treatment is shown in FIG. 4, and it is found that Al oxide is generated on the alpha-Fe phase, and Fe2The composite oxide of Cr-B is formed on the B phase.
After the alloy which is not subjected to the pre-oxidation treatment is corroded in the step (4) in the embodiment 1, a sample is subjected to hot sample embedding treatment, then sand paper grinding and polishing treatment are carried out, and then SEM surface morphology observation of a cross section is carried out, and as shown in a figure 3, the result that in a high-temperature zinc liquid, Fe-20Cr-5B-3Al alloy is corroded, an alpha-Fe phase is corroded firstly, and Fe which loses support is shown in a figure 32The phase B also gradually drifts into the zinc liquid. Sample after pre-oxidation treatment was subjected to the procedure of example 2After the corrosion in the step (5), after sample inlaying, grinding and polishing, cross-section SEM surface morphology observation is carried out, as shown in FIG. 4, it is found that after the sample preoxidized for 15h is corroded, an oxide layer shows transverse cracking and drifting, but the more internal oxide layer still blocks the corrosivity of zinc liquid to an alloy matrix; the sample after being pre-oxidized for 25h also shows excellent corrosion resistance; the sample preoxidized for 20 hours has the best corrosivity, and obvious cracks exist between the zinc liquid and the oxide layer, because the wettability of the oxide layer and the zinc liquid is poor, the zinc liquid only slightly erodes the oxide layer, further contact between the zinc liquid and the alloy matrix is blocked due to the existence of the oxide layer, and obvious corrosion does not occur on the matrix.
Comparative example 1:
different from the example 2, the pre-oxidation time is 5h, 10h and 30h respectively under the condition that the pre-oxidation temperature and the oxygen pressure are not changed. The method comprises the following steps of carrying out nickel plating, sample inlaying, grinding and polishing treatment on an oxidized sample, and then carrying out scanning electron microscope observation on a cross section, wherein the purpose of nickel plating is to distinguish sample inlaying resin from an oxide layer more easily on one hand, and play a role in protecting the oxide layer on the other hand. As shown in fig. 5, wherein (a) is a sectional view after 5h of pre-oxidation, and (b) is a sectional view after 10h of pre-oxidation, the oxide layer shows a tendency of gradually thickening along with the extension of the oxidation time, and the degree of internal oxidation of Al increases, and extends into the substrate in a tentacle shape. Then, the sample after being pre-oxidized for 10 hours is subjected to zinc liquid corrosion, and under the condition, although the oxide layer plays a certain role in blocking the zinc liquid, the corrosion phenomenon still occurs, and the zinc liquid diffuses in the matrix along the alpha-Fe phase, and the result is shown in a graph c. The surface of the sample after pre-oxidation for 30h is shown in figure d, and under the condition, the surface of the oxide layer has more gaps and peeling phenomena, and the surface does not play a role in blocking the zinc liquid.
Comparative example 2:
in contrast to example 2, at 900 ℃ and 10 ℃-16.8The result of 5h pre-oxidation treatment of the alloy under atm condition is shown in FIG. 6. Compare FIG. 5(a) at 850 ℃ and 10-20.5as a result of preoxidation for 5 hours under atm conditions, oxygen was foundThe thickness of the oxide layer is obviously increased to 40-50 μm, but the density of the oxide film is reduced, obvious holes and defects are formed in the oxide layer, and most of oxides of Fe are found through WDS energy spectrum, so that the oxide layer has no protection to a matrix.
However, the method for preparing the zinc liquid corrosion resistant FeCrBAl alloy is not limited to this, and those skilled in the art can select a suitable alloy smelting method, a vacuum oxidation device and an oxygen pressure according to actual engineering requirements, and specifically implement the method for preparing the zinc liquid corrosion resistant FeCrBAl alloy.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and their concepts should be equivalent or changed within the technical scope of the present invention.
Claims (7)
1. A preparation method of a FeCrBAL alloy resistant to zinc liquid corrosion is characterized by comprising the following steps: the method comprises the following steps:
(1) repeatedly smelting the chromium, the aluminum, the iron and the Fe-B intermediate alloy serving as raw materials by using a vacuum smelting furnace for 3-5 times, and carrying out vacuum annealing to obtain an iron-based alloy;
(2) carrying out surface treatment on the iron-based alloy by using a high vacuum tube furnace through a pre-oxidation method, wherein the pre-oxidation temperature is 800-850 ℃, and the oxygen pressure is 10-25atm～10-20atm and the oxidation time is 15-25 h.
2. The method for preparing a zinc liquid corrosion resistant FeCrBAl alloy according to claim 1, wherein the method comprises the following steps: the smelting times in the step (1) are 5 times.
3. The method for preparing a zinc liquid corrosion resistant FeCrBAl alloy according to claim 1, wherein the method comprises the following steps: in the step (1), the mass percentage of boron in the Fe-B intermediate alloy is 10-25%.
4. The method for preparing a zinc liquid corrosion resistant FeCrBAl alloy according to claim 1, wherein the method comprises the following steps: the mass percentage of the boron element in the Fe-B intermediate alloy in the step (1) is 20%.
5. The method for preparing a zinc liquid corrosion resistant FeCrBAl alloy according to claim 1, wherein the method comprises the following steps: in the step (1), the vacuum annealing temperature is 1000 ℃, and the annealing time is 72 h.
6. The method for preparing a zinc liquid corrosion resistant FeCrBAl alloy according to claim 1, wherein the method comprises the following steps: the iron-based alloy in the step (1) comprises 20% of chromium, 5% of boron, 3% of aluminum and the balance of iron in percentage by weight.
7. The method for preparing a zinc liquid corrosion resistant FeCrBAl alloy according to claim 1, wherein the method comprises the following steps: in the step (2), the pre-oxidation temperature is 850 ℃, and the oxygen pressure is 10-20.5atm and an oxidation time of 20 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101792884A (en) * | 2009-12-31 | 2010-08-04 | 首钢总公司 | Steel with underrelaxation and hydrogen corrosion resistance for high-speed railway prestressed pull rod and production method thereof |
| US20110265920A1 (en) * | 2008-12-09 | 2011-11-03 | Masaharu Hatano | High-purity ferritic stainless steels excellent in corrosion resistance and method of production of same |
| CN106854747A (en) * | 2016-12-29 | 2017-06-16 | 常州大学 | In a kind of low dew point environment Al containing zinc is prepared on Fe sills surface2O3And SiO2The method of film |
| CN108220804A (en) * | 2018-03-19 | 2018-06-29 | 北京工业大学 | The Cr-Al alloy Fe-B alloys and its manufacturing method of resisting zinc liquid corrosion abrasion |
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- 2021-10-18 CN CN202111210778.1A patent/CN113957327B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110265920A1 (en) * | 2008-12-09 | 2011-11-03 | Masaharu Hatano | High-purity ferritic stainless steels excellent in corrosion resistance and method of production of same |
| CN101792884A (en) * | 2009-12-31 | 2010-08-04 | 首钢总公司 | Steel with underrelaxation and hydrogen corrosion resistance for high-speed railway prestressed pull rod and production method thereof |
| CN106854747A (en) * | 2016-12-29 | 2017-06-16 | 常州大学 | In a kind of low dew point environment Al containing zinc is prepared on Fe sills surface2O3And SiO2The method of film |
| CN108220804A (en) * | 2018-03-19 | 2018-06-29 | 北京工业大学 | The Cr-Al alloy Fe-B alloys and its manufacturing method of resisting zinc liquid corrosion abrasion |
Non-Patent Citations (1)
| Title |
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| 王坤等: "低氧压预氧化对Fe-3Al-6Cr合金表面显微组织和耐蚀性影响", 《中国表面工程》 * |
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