CN113237821B - Preparation and detection method of yttrium-doped Inconel625 alloy applied to oxidative high-temperature chlorine corrosion environment - Google Patents
Preparation and detection method of yttrium-doped Inconel625 alloy applied to oxidative high-temperature chlorine corrosion environment Download PDFInfo
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- 239000000956 alloy Substances 0.000 title claims abstract description 82
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 80
- 229910001119 inconels 625 Inorganic materials 0.000 title claims abstract description 58
- 238000005260 corrosion Methods 0.000 title claims abstract description 54
- 230000007797 corrosion Effects 0.000 title claims abstract description 53
- 239000000460 chlorine Substances 0.000 title claims abstract description 29
- 229910052801 chlorine Inorganic materials 0.000 title claims abstract description 29
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 230000001590 oxidative effect Effects 0.000 title claims abstract description 16
- 238000001514 detection method Methods 0.000 title claims abstract description 8
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 16
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000000137 annealing Methods 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000003466 welding Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000005258 corrosion kinetic Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 7
- 239000010453 quartz Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 claims description 4
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- 238000004626 scanning electron microscopy Methods 0.000 claims description 3
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- 239000010813 municipal solid waste Substances 0.000 abstract description 8
- 238000013461 design Methods 0.000 abstract description 2
- 239000011651 chromium Substances 0.000 description 19
- 239000002245 particle Substances 0.000 description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 9
- 229910004298 SiO 2 Inorganic materials 0.000 description 6
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 229910001120 nichrome Inorganic materials 0.000 description 6
- 238000005204 segregation Methods 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000004056 waste incineration Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 230000004584 weight gain Effects 0.000 description 3
- 235000019786 weight gain Nutrition 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
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- 229910001510 metal chloride Inorganic materials 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229910052758 niobium Inorganic materials 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- G01N17/006—Investigating resistance of materials to the weather, to corrosion, or to light of metals
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
The invention belongs to the field of high-temperature chlorine corrosion resistant alloy design, and particularly relates to a preparation and detection method of yttrium-doped Inconel625 alloy applied to an oxidative high-temperature chlorine corrosion environment. (1) Taking an Inconel625 welding wire, carrying out ultrasonic cleaning together with yttrium, and drying to obtain a mixture; the mass fraction of yttrium in step (1) is taken as Inconel625: xY, the mass fraction x of yttrium taking on the values of 0.1 wt.%, 0.3 wt.%, 0.5 wt.%, 0.7 wt.% or 1.0 wt.%; (2) Performing arc melting on the mixture to obtain an alloy ingot, and annealing the alloy ingot to obtain yttrium-doped Inconel625 alloy; the invention aims to further improve the corrosion resistance of the Inconel625 which is commonly used in the high-temperature chlorine corrosion environment at present, and is more efficiently used in working scenes such as the surface of a heat exchanger tube bank of a garbage incinerator and the like.
Description
Technical Field
The invention belongs to the field of high-temperature chlorine corrosion resistant alloy design and performance test, and particularly relates to a preparation and detection method of yttrium-doped Inconel625 alloy applied to an oxidative high-temperature chlorine corrosion environment.
Background
In the high-temperature chlorine corrosion process of various metals and alloys, a protective corrosion layer cannot be formed due to the generation of metal chlorides with low melting point and high vapor pressure, and high economic loss and huge potential safety hazards are often accompanied in production and life. The high-temperature chlorine corrosion phenomenon, such as that occurring in the incineration process of garbage, has been receiving increasing attention and has been widely studied. With the increase of population base, environmental pollution caused by municipal solid waste in countries of the world is serious, the treatment of the municipal solid waste becomes a problem to be solved urgently, and although the popularization of classified recycling of the waste is gradually carried out in recent years, great effect is not seen. The waste incineration method can be used as a power plant to generate electricity due to the heat generated by the waste incineration method, so that the use of traditional fuels is reduced, and CO is reduced 2 The emission is beneficial to relieving the pressure of insufficient energy, and good social and economic benefits are achieved. The Incoenel625 nickel-based alloy shows good corrosion resistance in the environments of waste incineration boilers and biomass mixed coal combustion power generationBut its cost is very high. The corrosion resistance of the Inconel625 is further improved, the protection effect is exerted to a greater extent, the development of a waste incineration power generation technology is promoted, and the method plays an important role in the implementation of an advanced coal conversion technology. The addition of the element Y can better promote the protective Al of the outer layer 2 O 3 ，Cr 2 O 3 The formation of the layer improves the corrosion resistance of the alloy.
Disclosure of Invention
In order to achieve the expected aim, the invention provides a preparation method and a detection method of yttrium-doped Inconel625 alloy applied to an oxidative high-temperature chlorine corrosion environment. Yttrium-doped Inconel625 alloy (Inconel 625: xY, x =0,0.1,0.3,0.5,0.7,1.0 wt.%) was prepared using high-purity yttrium metal particles (99.99%) and Inconel625 welding wire as starting materials using vacuum arc melting technique and examined in an oxygen-containing HCl atmosphere (N: (N)) 2 -0.5 % HCl-1.5 % O 2 -3.0 % CO 2 ) Corrosion behavior at the temperature of 600-800 ℃. The alloy material is used as a high-temperature chlorine corrosion resistant alloy material with high cost performance, and is expected to be applied to the surface of a heat exchanger tube bank of a garbage incinerator to prepare a corrosion-resistant coating.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of yttrium-doped Inconel625 alloy applied to an oxidative high-temperature chlorine corrosion environment comprises the following steps:
(1) Taking an Inconel625 welding wire, carrying out ultrasonic cleaning on the Inconel625 welding wire and yttrium together, and drying to obtain a mixture;
the mass fraction of yttrium in step (1) is taken as Inconel625: xY, the mass fraction x of yttrium taking on the values of 0.1 wt.%, 0.3 wt.%, 0.5 wt.%, 0.7 wt.% or 1.0 wt.%;
(2) And arc melting the mixture to obtain an alloy ingot, and annealing the alloy ingot to obtain the yttrium-doped Inconel625 alloy.
Further, in the step (1) above: preferred values for the mass fraction x of yttrium are: x =0.1 wt.
Further, in the step (2) above: the arc melting condition is one atmosphere of argon, and the current range is 180-220A.
Further, in the step (2) above: the annealing of the alloy ingot is performed at 900 ℃ for an annealing time of 24 h.
Further, wire cutting, grinding and polishing are performed after the alloy ingot is annealed.
A detection method of yttrium-doped Inconel625 alloy applied to an oxidative high-temperature chlorine corrosion environment comprises the following steps:
detecting the corrosion resistance behavior of the prepared yttrium-doped Inconel625 alloy in an oxidative high-temperature chlorine corrosion environment;
the oxygen-containing high-temperature chlorine corrosion environment is N 2 -0.5 % HCl-1.5 % O 2 -3.0 % CO 2 600-800 ℃, and the corrosion time is 200 h.
Further, the detection method comprises the following steps:
(1) Weighing the prepared yttrium-doped Inconel625 alloy, and measuring the accurate size by using a vernier caliper;
(2) Putting the prepared yttrium-doped Inconel625 alloy into a quartz crucible, putting the crucible into a quartz tube, and introducing N 2 、CO 2 Heating the furnace to a corresponding temperature at a speed of 4 ℃/min, introducing HCl, preserving the temperature by 10 h, and turning off HCl and CO 2 And taking out the alloy after furnace cooling, weighing, repeating the operation until the corrosion is finished by 200 h to obtain a corrosion kinetic curve, and carrying out surface SEM/EDS analysis on the corroded sample.
Compared with the prior art, the invention has the beneficial effects that:
at present, the industrial production of the inner wall coating of the garbage incinerator is mainly to prepare the nickel-based coating by adopting a surfacing technology, and a certain corrosion resistance is obtained, but the cost is higher. In the present invention, the addition of 0.1 wt.% and 0.3 wt.% Y significantly improves the high temperature chlorine corrosion resistance of Inconel625 alloy because the addition of 0.1 wt.% and 0.3 wt.% Y can rapidly promote Cr 2 O 3 The protective layer is formed on the surface of the alloy substrate, and the effect thereof becomes more remarkable as the temperature increases. The modified Inconel625:0.1Y alloy prepared by the method forms continuous and compact Cr 2 O 3 Layer of 200 h corrosion weight gain onlyThe alloy is 23.62 percent of unmodified Inconel625 alloy, shows better corrosion resistance, and achieves the expected aims of further improving the corrosion resistance of the Inconel625 which is commonly used in the high-temperature chlorine corrosion environment at present and more efficiently serving working scenes such as the surface of a heat exchanger tube bank of a garbage incinerator.
Drawings
FIG. 1 is a flow chart of the manufacturing process of the present invention;
FIG. 2 is a graph of the corrosion kinetics of an Inconel625: xY (x =0,0.1,0.3,0.5,0.7,1.0 wt%) alloy of the present invention at 700-800 ℃ and 200 h;
FIG. 3 is a graph of the corrosion kinetics of the Inconel625, inconel625:0.1Y, inconel625:0.3Y alloys of the invention at 600-800 ℃ and 200 h;
FIG. 4 shows an Inconel625: xY (x =0,0.1,0.3,0.5,0.7,1.0 wt%) alloy at 600 ° C, N 2 -0.5 % HCl-1.5% O 2 -3.0% CO 2 Surface morphology after etching 200 h in mixed atmosphere: inconel625 (b), inconel625-0.1Y (c), inconel625-0.3Y (d), inconel625-0.5Y (e), inconel625-0.7Y (f), inconel625-1.0Y 1, enlarged view 2: full view;
FIG. 5 shows an Inconel625: xY (x =0,0.1,0.3,0.5,0.7,1.0 wt%) alloy of the present invention at 700 ° C, N 2 -0.5%HCl-1.5%O 2 -3.0%CO 2 Surface morphology after etching 200 h in mixed atmosphere: inconel625 (b), inconel625-0.1Y (c), inconel625-0.3Y (d), inconel625-0.5Y (e), inconel625-0.7Y (f), inconel625-1.0Y 1, enlarged view 2: full view;
FIG. 6 shows Inconel625: xY (A-Y) according to the inventionx=0,0.1,0.3,0.5,0.7,1.0 wt%) alloy at 800 ° C, N 2 -0.5%HCl-1.5%O 2 -3.0%CO 2 Surface morphology after etching 200 h in mixed atmosphere: inconel625 (b), inconel625-0.1Y (c), inconel625-0.3Y (d), inconel625-0.5Y (e), inconel625-0.7Y (f), inconel625-1.0Y 1, enlarged view 2, full view.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to the following examples. The process is conventional unless otherwise specified, and the starting materials are commercially available from the open literature.
FIG. 1 is a flow chart of the preparation process of the present invention.
Firstly, cutting an Inconel625 welding wire to be convenient for subsequent weighing, weighing relatively excessive yttrium particles, separately carrying out ultrasonic cleaning and drying on the two, and then weighing the components in specified weight: inconel625 xY (Ixol: (Ixol) (Ixol))x=0, 0.1, 0.3, 0.5, 0.7, 1.0 wt%)。
Secondly, arc melting under argon protection is carried out, and the melting environment is as follows: argon gas is under 1 atmosphere, current is 200A, alloy button ingots are obtained, annealing is carried out on the alloy at 900 ℃ for 24 h, the alloy is subjected to wire cutting to be 10 multiplied by 1 mm samples, and grinding and polishing are carried out.
Secondly, the sample is subjected to high-temperature chlorine corrosion performance test. High temperature chlorine corrosion test: the sample was weighed and a vernier caliper measured the exact dimensions. Putting the sample into a quartz crucible, putting the crucible into a quartz tube, and introducing N 2 、CO 2 Heating the furnace to a corresponding temperature at a speed of 4 ℃/min, introducing HCl, preserving the temperature by 10 h, and turning off HCl and CO 2 And taking out the sample after the sample is cooled along with the furnace, weighing, and repeating the operation until the corrosion is finished at 200 h to obtain a corrosion kinetic curve (figures 2 and 3). Surface SEM/EDS analysis was performed on the post-corrosion samples (fig. 4, 5, 6).
Available from corrosion kinetics, inconel625-xY(x=0,0.1,0.3,0.5,0.7,1.0 wt.%) six alloys at 700-800 ° C, N 2 -0.5 vol.% HCl-1.5 vol.% O 2 -3.0 vol.% CO 2 After 200 h is corroded in the corrosive atmosphere, the weight of the whole alloy is increased. At 700 ℃, the addition of Y does not appear to improve the corrosion resistance of the alloy, the corrosion kinetics curve of the Inconel625-0.1Y alloy almost coincides with that of the Inconel625 alloy, and the corrosion rate of the Inconel625-0.7Y alloy is much higher than that of the other alloys. With increasing temperature, the corrosion kinetics curve of the alloy at 800 ℃ approximately follows a parabolic law. Wherein the corrosion weight gain of Inconel625-0.1Y and Inconel625-0.3Y alloys is lower than that of Inconel625 alloy, especially the addition of 0.1 wt% Y, and the corrosion resistance is better, and the corrosion weight gain of 200 h is only unchanged23.62% of the sex Inconel625 alloy.
From the surface morphology and the composition analysis, at 600 ℃, inconel625-xY(x=0,0.1,0.3,0.5,0.7,1.0 wt.%) the alloy formed very similar oxide films with small amounts of mixed oxides of Ni, cr on the surface. The surface of the Inconel625 alloy is subjected to Nb aggregation, the Inconel625-xY(x=0,0.1,0.3,0.5,0.7,1.0 wt%) segregation of Y occurs at the white particles of the alloy. 700. The Inconel625 alloy surface is mainly formed by Cr at the temperature of DEG C 2 O 3 And NiCr 2 O 4 The white particles are Cr 2 O 3 (ii) a The surface of the Inconel625-0.1Y alloy is mainly composed of Cr 2 O 3 And NiCr 2 O 4 Forming; the surface of the Inconel625-0.3Y alloy is mainly composed of Cr 2 O 3 ， NiCr 2 O 4 And SiO 2 The white particles are Cr 2 O 3 . As the Y content increases, the Si content on the surface of the alloy also increases. The surface of the Inconel625-0.5Y alloy is mainly composed of Cr 2 O 3 ，NiCr 2 O 4 And SiO 2 The white particles are mixed oxides of Si and Cr. The surface of the Inconel625-0.7Y alloy is mainly made of SiO 2 Composition, segregation of Y occurred at white particles (point a), with about 4 wt% Cl detected. At 800 ℃, the Inconel625 alloy surface is mainly formed into Cr 2 O 3 ，SiO 2 And part of simple substance Ni. EDS analysis shows higher Si content in the dark areas and higher Ni content in the light areas. The surfaces of the Inconel625-0.1Y and Inconel625-0.3Y alloys form white Cr 2 O 3 The particles, the dark surface of which contains part of the Ni, have a skinning phenomenon observed on the surface of the Inconel625-0.3Y alloy due to the effects of thermal and internal stresses. The Inconel625-0.5Y alloy surface forms relatively continuous Cr 2 O 3 Segregation of Y and Nb occurs at the white particles of the layer. The surface of the Inconel625-0.7Y alloy consists essentially of Cr 2 O 3 And NiCr 2 O 4 Composition and containing a small amount of SiO 2 The white particles are Cr 2 O 3 And segregation of Y occurs at the white particles. The Inconel625-1.0Y alloy mainly grows Si and Cr mixed oxides on Ni, si and Cr mixed oxidesOxide: cr (chromium) component 2 O 3 ，NiCr 2 O 4 And SiO 2 White particles show segregation of Y.
The modified Inconel625:0.1Y alloy prepared by the method forms continuous and compact Cr 2 O 3 The layer shows better corrosion resistance, achieves the expected target of further improving the corrosion resistance of the Inconel625 which is commonly used in the high-temperature chlorine corrosion environment at present and is more efficiently used in working scenes such as the surface of a heat exchanger tube bank of a garbage incinerator and the like.
The foregoing is only a preferred embodiment of the present invention and it should be noted that modifications and adaptations can be made by those skilled in the art without departing from the principle of the present invention and are intended to be included within the scope of the present invention.
Claims (6)
1. A preparation method of yttrium-doped Inconel625 alloy applied to an oxidative high-temperature chlorine corrosion environment is characterized by comprising the following steps:
(1) Taking an Inconel625 welding wire, carrying out ultrasonic cleaning together with yttrium, and drying to obtain a mixture;
in the step (1), the mass fraction of yttrium is 0.1 wt% according to Inconel625: xY and the mass fraction x of yttrium;
(2) And arc melting the mixture to obtain an alloy ingot, and annealing the alloy ingot to obtain the yttrium-doped Inconel625 alloy.
2. The method for preparing the yttrium-doped Inconel625 alloy applied to the oxidative high-temperature chlorine corrosion environment according to claim 1, wherein the method comprises the following steps:
in the above step (2): the arc melting condition is one atmosphere of argon, and the current range is 180-220A.
3. The method for preparing the yttrium-doped Inconel625 alloy applied to the oxidative high-temperature chlorine corrosion environment according to claim 1, wherein the method comprises the following steps:
in the above step (2): the annealing of the alloy ingot is performed at 900 ℃ for an annealing time of 24 h.
4. The method for preparing the yttrium-doped Inconel625 alloy applied to the oxidative high-temperature chlorine corrosion environment according to claim 3, wherein the method comprises the following steps: and performing wire cutting, grinding and polishing after annealing the alloy ingot.
5. The method for detecting the yttrium-doped Inconel625 alloy applied to the oxidative high-temperature chlorine corrosion environment according to claim 1, wherein the method comprises the following steps:
detecting the corrosion resistance behavior of the prepared yttrium-doped Inconel625 alloy in an oxidative high-temperature chlorine corrosion environment;
the oxidative high-temperature chlorine corrosion environment is N 2 -0.5 % HCl-1.5 % O 2 -3.0 % CO 2 600-800 ℃, and the corrosion time is 200 h.
6. The method for detecting the yttrium-doped Inconel625 alloy applied to the oxidative high-temperature chlorine corrosion environment according to claim 5, wherein the detection method comprises the following steps:
(1) Weighing the prepared yttrium-doped Inconel625 alloy, and measuring the accurate size by using a vernier caliper;
(2) Putting the prepared yttrium-doped Inconel625 alloy into a quartz crucible, putting the crucible into a quartz tube, and introducing N 2 、CO 2 Heating the furnace to a corresponding temperature at a speed of 4 ℃/min, introducing HCl, preserving the temperature by 10 h, and turning off HCl and CO 2 And taking out the alloy after furnace cooling, weighing, repeating the operation until the corrosion is finished by 200 h to obtain a corrosion kinetic curve, and carrying out surface SEM/EDS analysis on the corroded sample.
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