AU2019422376B9 - Modified austenitic stainless steel having good high-temperature creep resistance performance and preparation method therefor - Google Patents
Modified austenitic stainless steel having good high-temperature creep resistance performance and preparation method therefor Download PDFInfo
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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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/74—Methods of treatment in inert gas, controlled atmosphere, vacuum or pulverulent material
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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
- C21D10/00—Modifying the physical properties by methods other than heat treatment or deformation
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/02—Pretreatment of the material to be coated
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/36—Embedding in a powder mixture, i.e. pack cementation only one element being diffused
- C23C10/48—Aluminising
- C23C10/50—Aluminising of ferrous surfaces
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/60—After-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F3/00—Electrolytic etching or polishing
- C25F3/16—Polishing
- C25F3/22—Polishing of heavy metals
- C25F3/24—Polishing of heavy metals of iron or steel
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Abstract
A modified austenitic stainless steel having a good high-temperature creep resistance performance and a preparation method therefor. Said modified steel comprises a steel substrate and a percolation layer, the percolation layer comprising, from inside to outside, a 40-80μm of Fe-phase diffusion layer containing Al, a 50-100μm of Fe-Al compound layer, and a 10-20μm of Al
Description
The present invention relates to the technical field of heat exchange tube materials, in
particular to a modified austenitic stainless steel with excellent high-temperature creep
resistance and a preparation method therefor.
Solar thermal power (also called concentrating solar power, CSP), as a representative of
clean energy, has been appreciated extensively during energy structure optimization because
of having stable, continual and controllable power output and being capable of realizing the
advantages of complementation with photovoltaic power and wind power. A thermal storage
system is a vital link of a CSP station. Recently, vapor, molten salt and conduction oil are
mainly applied as thermal storage media for the commercial CSP stations. Due to such
features as low thermal storage capacity of the vapor, low thermal conductivity, easy
decomposition and solid-liquid layering of the molten salt at high temperature, and easy
decomposition of the conduction oil at high temperature (over 400°C), the thermal storage
system has the defects of low thermal conduction efficiency, poor thermal stability, high
degree of supercooling, and the like, thereby leading to high power generation cost and
limiting the development of solar thermal power. For an aluminum-silicon (Al-Si) alloy, the
latent heat may be 960 J/g at 1,079°C, the thermal conductivity is more than twice that of the
salt, the phase change latent heat decreases to 452 kJ/kg from 505 kJ/kg with a decreasing
amplitude of 10.5% after 720 melting-solidification cycles at the melting point of 575°C, and
the phase change temperature remains stable essentially. With a feature of high oxidation
resistance (the oxidation ratio is less than 0.01% after hundreds of hours of high temperature
oxidation), the Al-Si alloy is considered as a new generation of substitute material for the
thermal storage medium.
However, in practical applications, the working conditions and application environments
of heat exchange tube fittings for the solar thermal power are extremely severe, including bearing a constant high stress load and temperature fluctuation between 495C and 620'C, being corroded by the molten Al-Si alloy as the thermal storage medium, and being damaged by corrosion creep deformation to further shorten the service life of the thermal power system.
Hence, it is an urgent problem to be solved during CSP research and development to improve
the high-temperature creep resistance against the molten Al-Si alloy of the heat exchange tube
materials. At present, the method of slowing the corrosion caused by the molten Al-Si alloy is
to aluminize the austenitic stainless steel for the heat exchange tubes. Aluminizing, as a
mature chemical heat treatment process, has been extensively used in industrial production.
Nevertheless, in the ordinary aluminizing process, the phase composition of the aluminized
coating surface is uneasily controlled; the brittle phase is produced easily; the aluminized
coating is usually too thin and loose, is bound to the substrate un-tightly and stripped easily,
which affects the surface strengthening effect, or reduces the strength and toughness of the
materials during the treatment. As can be seen, the aluminized steel prepared by the existing
aluminizing process still has distinct disadvantages in terms of mechanical property. For
example, the aluminized specimen shows a higher creep strain rate and a shorter creep rupture
life due to low bearing capability of the aluminized layer, insufficient material toughness and
strength as well as easy nucleation and rapid expansion of micropores or microcracks in the
aluminized coating.
Laser shock peening is an advanced surface enhancement technology capable of refining
surface material grains, improving dislocation density, introducing higher residual
compressive stress, and effectively restraining crack initiation and extension to improve the
mechanical property of the materials. However, each material, subject to the joint treatment of
aluminization and laser shock, has the problems that the surface roughness increases, the
coating is easily stripped, the generated aluminized layer cracks easily under a
high-temperature load, and the life of workpiece is shortened. For example, the patent
(application No.: 201310282671.7) discloses a composite treatment method by aluminization
and laser shock, involving the technological processes of pre-cleaning, annealing for 2~3 h at
550~780°C, shot blasting, aluminizing for 4~6 h at 500~600'C, post cleaning and final laser
shock. The aluminized coating generated by such process consists of Fe 2Al 5 brittle phase as
main component, which does not solve the problem of brittleness of the aluminized coatings.
Moreover, the coatings are easily stripped in laser shock, and the binding force between the
aluminized coating and the substrate is poor, so that the residual compressive stress
introduced by the laser shock peening at high temperature can be greatly released, and an
enhancement effect of fretting-fatigue resistance is poor.
The document Study on Aluminizing Process of CrlNiWMoV Steel after Laser Shock
Peening (Chinese Journal of Lasers, 2011, 38 (7), 126~130) discloses a method for
aluminizing for 12 h at 510°C after laser shock peening. Due to lower aluminizing
temperature, the process can effectively prevent the residual compressive stress introduced by
virtue of laser shock peening from releasing, and thus does not affect the aluminizing
thickness. However, the main component of the aluminized coating is FeA13 brittle phase, so
that the cracks are easily nucleated on the aluminized coating and the residual compressive
stress is greatly released after loading at high temperature, thereby leading to poor
enhancement effect of the mechanical property at high temperature. The patent (application
No.: 20111006570.2) discloses a method of first laser shock, then aluminizing and finally
laser shock. The aluminized coating obtained by the method is easily stripped during the laser
shock, the aluminizing thickness is affected, the process is fussy, the treatment period is long,
and the production cost is high.
The heat exchange tube for solar thermal power, that takes the Al-Si alloy as the thermal
storage medium, requires high creep resistance in an application environment of the molten
Al-Si alloy at high temperature (620°C). In a patent (application No. 201310282671.7), the
compressive residual stress can be introduced to the surface of the aluminized layer to provide
the surface strength, but the binding force of the aluminized coating obtained is not strong.
Also, due to the Fe 2A 5 brittle phase included in the aluminized coating, the strengthening
effect at high temperature is too poor to meet the requirement for operation of the heat
exchange tube for a long time when the compressive residual stress greatly releases at high
temperature.
In view of the foregoing defects of the above technology, the technical problem to be
solved by the present invention is to provide a new process for joint treatment by
aluminization and laser shock. Through such process, a modified austenite, with uniform
structure, strong binding force of the aluminized coating and toughened surface-strengthened substrate and no brittle phase, can be obtained to ensure that the heat exchange tube is excellent in high-temperature creep resistance. SUMMARY The technical problem to be solved by the present invention is to overcome the defects of the prior art, that is to say, to provide a modified austenitic stainless steel with excellent creep and corrosion resistance in the case of the molten Al-Si alloy, strong binding force between the aluminized coating and the substrate, good anti-strip performance, good toughness and strength and no brittle phase in components of the aluminized coatings, and to further provide a simple method for preparing the modified austenitic stainless steel with strong binding force between the aluminized coating and the substrate, good anti-strip performance, excellent high-temperature creep resistance and corrosion resistance in the case of the molten Al-Si alloy, good toughness and strength and no brittle phase. To solve the aforesaid technical problems, the technical solution applied by the present invention is as follows: A modified austenitic stainless steel with the excellent high-temperature creep resistance, the modified austenitic stainless steel comprising an austenitic stainless steel substrate and aluminized coating, wherein the aluminized coating, from inside to outside, comprising an Al-containing Fe phase diffusion layer with a thickness of 40~80 p m, a Fe-Al compound layer with a thickness of 50-100 P m and anA1 20 3 film with a thickness of 10~20 Pm. According to the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, the Fe-Al compound layer is non-brittle intermetallic compounds of Fe and Al; the non-brittle intermetallic compounds comprise FeAl, FeAl 2 and Fe 3Al. According to the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, the austenitic stainless steel substrate is 321 austenitic stainless steel; the surface hardness of the aluminized coating is 625~1,390 HV, and the strengthening depth is 300~1,600 P m. As an overall inventive concept, the preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance is further provided, comprising the following steps: SI. electrolytic polishing: electrolytically polishing an austenitic stainless steel plate by taking the austenitic stainless steel plate as an anode and an insoluble conducting material as a cathode; S2. aluminizing: drying the austenitic stainless steel after being electrolytically polished, aluminizing using a solid powder aluminizing medium, wherein the aluminizing conditions include: first holding for 20~40 min at 400~600°C, and then conducting furnace cooling to room temperature after holding for 10~15 h at 900~1,050°C; S3. sand-blasting treatment: conducting sand-blasting for the specimen aluminized under 0.6~0.9 MPa high pressure nitrogen; S4. annealing: annealing the specimen after being subject to sand-blasting treatment in an argon atmosphere at 1,000~1,100°C, and taking out the specimen after furnace cooling; and S5. laser shock peening: conducting laser shock treatment for the specimen after being annealed, wherein the single pulse energy of the laser shock is 4-7 J, the spot diameter is 2.6~3 mm, the number of laser shocks is 1~3; and obtaining the modified austenitic stainless steel after the laser shock peening treatment. According to the aforesaid preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, in the step S2, the solid powder aluminizing medium is a uniform mixture of the following components: an aluminium powder with a particle size of 200 meshes, a filler consisting of an A1 2 0 3 and a Cr powder and a powder NH 4 Cl as a permeation promoter; in the solid powder aluminizing medium, by mass ratio, the aluminium powder is 42~74%, the A12 0 3 powder is 20~40%, the Cr powder is 5~15%, and the NH 4 C is 1~3%. According to the preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, in the step S4, the annealing time is 0.5-3 h.
According to the preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, in the step S5, a pulse high-energy laser device is applied, a black tape is taken as a protective layer, and water is taken as a restraint layer; the laser has a wave length of 1,064 nm, a pulse width of 10~30 ns, and an overlap rate of 40~70%; the laser shock treatment is a double-sided laser shock treatment; the path direction of the laser shock treatment is vertical to the rolling direction of the stainless steel plate. According to the preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, in the step S3, the sand-blasting abrasive is A12 0 3 particles with 300500 meshes; the sand-blasting time is 5-20 min, and the sand-blasting distance is 2~6 cm. According to the preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, in the step Sl, the electrolyte comprises concentrated sulfuric acid with a volume fraction of 60~80%, concentrated phosphoric acid with a volume fraction of 15~37% and distilled water with a volume fraction of 3~5%; the electrolytic DC voltage is 5-6 V, the temperature of the electrolyte is 6080°C, and the electrolytic polishing time is 2~5 min. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance, preferably, prior to the step S1, further comprising a step of conducting surface mechanical polishing treatment for the austenitic stainless steel; the specific steps of the surface mechanical polishing include: grinding to remove visible scratches using an abrasive paper with the particle size varying from 80 to 1,200 meshes, ultrasonically cleaning for 5~20 min in acetone to remove oil, and then ultrasonically cleaning for 5~20 min in absolute ethyl alcohol to remove stains, and finally drying in a drying oven for 20~40 min at 80°C. Compared with the prior art, the present invention has the following advantages: 1. The modified austenitic stainless steel provided by the present invention has excellent creep resistance and high material strength and toughness in the case of molten Al-Si alloy and high-temperature stress due to an excellent structure thereof. On the surface of the stainless steel substrate, from inside to outside, sequentially comprises the Al-containing Fe phase diffusion layer with the thickness of 40~80 m, the Fe-Al compound layer with the thickness of 50~100 m and the A1 2 0 3 film with the thickness of 10~20 m. The aluminized coating, without the brittle phases, has a uniform structure and a controllable thickness, and gradiently and smoothly transitive components between the layers, thereby significantly lowering the interfacial stress and structural defects between the substrate and the aluminized coating, effectively improving the binding force between the substrate and the aluminized coating, restraining the stripping and crack initiation & extension of the aluminized coating, effectively improving the creep resistance of the 321 austenitic stainless steel in the case of the molten Al-Si alloy and the high temperature stress, meeting the working demand of the heat exchange tube for solar thermal power based on the molten Al-Si alloy as the thermal storage medium, and having a great academic value and an industrial application potential. 2. The aluminized coating of the modified austenitic stainless steel provided by the present invention does not comprise brittle phases such as Fe 2Al 5 and FeA1 3, has a strong bearing capacity and a good adhesiveness between the aluminized coatings and between the aluminized coating and the substrate, and thus is stripped uneasily. 3. The aluminized coatings of the modified austenitic stainless steel provided by the present invention are bonded tightly with obvious boundaries and no cracks, the surface hardness of the aluminized coating is 625~1,390 HV, the strengthening depth is 300~1,600
[tm, and the surface strengthening effect of the material is good. 4. According to the present invention, the 321 stainless steel is treated by sequentially binding these processes including specific electrolytic polishing, aluminizing, sand-blasting, annealing and laser shock peening, and such parameters as aluminizing temperature, sand-blasting pressure, annealing temperature, laser shock path, single pulse energy and spot strength are controlled, thus its aluminized coating is obtained. The aluminized coating comprises, from outside to inside, the A1 2 0 3 film with a thickness of 10~20 m, the Fe-Al compound layer (FeAl, FeA 2 and Fe 3Al) with a thickness of 50~100 tm and the Al-containing Fe phase diffusion layer (the Al-containing Fe phase diffusion layer) with a thickness of 40~80 m sequentially. The aluminized coating has such advantages of tight binding between the aluminized layers, obvious and regular boundaries, small stress between interfaces, small interfacial stress between the substrate and the aluminized coating, good macro appearance of the aluminized coating, fine crystal particles, uniform structures, controllable thickness, gradient and smooth transition of the components between the aluminized layers, and without fissures, cracks and such brittle phases as Fe 2Al 5 and FeA13 ,
significantly lowering the interfacial stress and structure defects between the substrate and the aluminized coating, effectively improving the binding force between the substrate and the aluminized coating, restraining the stripping of the aluminized coating and the crack initiation
& extension, and effectively improving the creep resistance of the 321 stainless steel in the
case of the molten Al-Si alloy and the high temperature pressure. Such that the modified 321
stainless steel has an excellent creep resistance in the case of the molten Al-Si alloy and the
high temperature pressure, and is capable of improving the strength and toughness of the
austenitic stainless-steel substrate.
5. According to the method provided by the present invention, the regulation precision of
the structure can be further improved by further controlling such process parameters as
annealing time, aluminizing medium composition, process parameters of laser shock,
sand-blasting time, sand-blasting distance and conditions of electrolytic polishing, thereby
further improving the structure compactness and integrity, obtaining the modified austenite
with high surface strengthening and high substrate toughness, and effectively improving the
creep resistance, toughness and strength of the modified austenitic stainless steel in the case
of molten Al-Si alloy and high temperature stress.
6. According to the method provided by the present invention, the austenitic stainless
steel specimen is subject to surface mechanical polishing before being electrolytically
polished, thus removing impurities and coverings from the specimen surface, improving the
cleanliness of the specimen surface, and creating a good surface condition for the subsequent
aluminizing treatment.
Fig. 1 is a diagram of the laser shock peening path of conducting laser shock treatment
for the austenitic stainless-steel specimen provided by the present invention.
Fig. 2 is a XRD diagram of comparing the modified 321 austenitic stainless steel
obtained in Embodiment 3 of the present invention with the unmodified 321 austenitic
stainless steel.
Fig. 3 are a section appearance diagram of a modified 321 austenitic stainless steel
obtained in Embodiment 3 of the present invention and EDS energy spectrum analysis
diagrams for corresponding points thereof.
Fig. 4 is a microhardness changing diagram of a modified 321 austenitic stainless steel
obtained in Embodiment 3 of the present invention in the aluminized coating depth direction.
Fig. 5 is a high-temperature creep curve diagram of comparing the modified 321
austenitic stainless steel obtained in Embodiment 3 of the present invention with the
unmodified 321 austenitic stainless steel under 620°C/21OMPa and in the melting Al-Si alloy
environment under 620°C/21OMPa.
The present invention will be further explained in detail in combination with the
drawings and specific embodiments.
A modified austenitic stainless steel with excellent high-temperature creep resistance
provided by the present invention, the modified austenitic stainless steel comprising, from
inside to outside, an austenitic stainless steel substrate, an Al-containing Fe phase diffusion
layer with a thickness of 40~80 m, a Fe-Al compound layer with a thickness of 50~100 m
and an A1 2 0 3 film with a thickness of 10~20 m.
The Fe-Al compound layer is non-brittle intermetallic compounds of Fe and Al, which
comprises FeAl, FeAl 2 and Fe 3Al.
The austenitic stainless steel substrate is 321 austenitic stainless steel.
A preparation method for the modified austenitic stainless steel with excellent
high-temperature creep resistance provided by the present invention, comprising the
following steps:
(1) surface mechanical polishing: polishing a hot rolled austenitic stainless steel plate
to remove visible scratches using an abrasive paper with different particle sizes (80-1,200#) ,
ultrasonically cleaning for 5~20 min in acetone to remove oil, and then ultrasonically cleaning
for 5~20 min in absolute ethyl alcohol to remove stains, and finally drying in a drying oven
for 20-40 min at 80°C, wherein the 321 austenitic stainless steel is a rolled plate, and
comprises the following chemical components (by mass fraction): 0.04% of C, 0.38% of Si,
1.08% of Mn, 17.02% of Cr, 9.06% of Ni, 0.05% of N, 0.03% of P, 0.22% of Ti and the rest
of Fe; the mechanical properties of the 321 stainless steel at room temperature are as follows:
the tensile strength (ab) is 667 MPa, the yield strength (ao.2) is 245 MPa, the elongation is
56.5% and the hardness is 175 HV;
(2) electrolytic polishing: connecting the 321 austenitic stainless steel plate to an
anode at a distance of 50 mm from a cathode made of an insoluble conducting material
(graphite plate); heating an electrolyte to 60~80°C (optionally, heating in water bath);
switching on 5-6V DC voltage and taking out the austenitic stainless steel plate for rinsing
and drying after polishing for 2-5 min in electrolysis, wherein the electrolyte comprises the
following components (by volume fraction): 60-80% of concentrated sulfuric acid (98% pure),
15-37% of concentrated phosphoric acid (85% pure) and 3-5% of distilled water;
(3) aluminizing: the solid powder aluminizing medium consists of an aluminium
source, a filler and a permeation promoter (activator), wherein aluminium powder with the
particle size of 200 meshes is taken as the aluminium source, A1 2 0 3 and Cr powder as the
filler and powder NH 4 Cl as the permeation promoter, all of which are fully mixed based on
5~15 wt.% of Cr, 42~74 wt.% of Al, 20~40 wt.% of A1 2 0 3 and 1~3 wt.% of NH 4 Cl; placing
the aluminizing medium and the electrolytically polished austenitic stainless steel plate into a
heat-resistance stainless steel tank, compressing, and sealing with a refractory mortar for
aluminizing: conducting furnace heating, drying for 2 h at 150°C, holding for 20~40 min at
400~600°C at a heating rate of10C/min, and conducting furnace cooling to room
temperature after holding for 10~15 h at 900~1,050°C;
(4) sand-blasting treatment: sand-blasting the austenitic stainless-steel plate
aluminized under 0.6~0.9 MPa high pressure nitrogen to remove the loose aluminized
coatings and impurities, wherein the abrasive is A1 2 0 3 particles with 300-500 meshes, the
sand-blasting time is 5~20 min, and the sand-blasting distance is 2~6 cm.
(5) annealing: placing the aluminized austenitic stainless-steel plate into a vacuum
tube furnace, annealing for 0.5~3 h under a high pure argon at 1,000~1,100°C, and taking out
after furnace cooling.
(6) laser shock peening: conducting double-sided laser shock peening treatment for
the annealed austenitic stainless-steel plate, wherein the laser wave length is 1,064 nm, the
single pulse energy is 4-7 J, the pulse width is 10-30 ns, the spot diameter is 2.6-3 mm, the
overlap rate is 40-70%, the black tape is a protective layer, water is a restraint layer, and the
number of laser shocks is 1~3 (may be 1, 2 or 3). Fig. 1 is the laser shock peening path which
is vertical to the rolling direction of the stainless-steel plate.
According to the modified austenitic stainless steel with the enhanced high-temperature
creep resistance against the molten Al-Si alloy and the preparation method therefor, the aluminized coating has a good surface macro appearance and fine crystal grains without cracks after the austenitic stainless steel is aluminized and laser shocked. The aluminized coating, of a multi-layer structure, includes an uneven A1 2 0 3 film with a thickness of 10~20
[tm, a Fe-Al compound (FeAl, FeAl2 and Fe 3Al) with a thickness of 50~100 m, and an Al(Fe)-containing phase diffusion layer with a thickness of 40~80 m and a substrate sequentially from outside to inside. Moreover, the aluminized layers are bound tightly, with obvious and regular boundaries and no cracks. The surface hardness of the aluminized coating is 625~1,390 HV, and the strengthening depth is 300~1,600 [m. Under the molten Al-Si alloy environment at 620°C, the high-temperature tensile creep rupture time is more than 94 h under the 210 MPa creep load, and the steady-state creep rate is below 1.1254X 10- ; compared with the 321 stainless steel (the tensile creep rupture time is 73 h, and the steady-state creep rate is 2.7143 X 10-7), the steady-state creep rate is greatly reduced, the excellent high-temperature creep resistance against the molten Al-Si alloy is shown, an operating demand of the heat exchange tube for solar thermal power based on the molten Al-Si alloy as the thermal storage medium can be met, and thus the great academic value and industrial application potential are realized. Embodiment 1: A preparation method for the modified austenitic stainless steel with excellent high-temperature creep resistance provided by the present invention, comprising the following steps: (1) surface mechanical polishing: polishing a hot-rolled austenitic stainless steel plate specimen to remove visible scratches using an abrasive paper with different particle sizes (80 to 1,200 meshes), ultrasonically cleaning the specimen in acetone for 5 min to remove the oil, and then ultrasonically cleaning for 5 min in absolute ethyl alcohol to remove stains, and finally drying in a drying oven for 20 min at 80°C; wherein the 321 austenitic stainless steel is a rolled plate, and comprises the following chemical components (by mass fraction): 0.04% of C, 0.38% of Si, 1.08% of Mn, 17.02% of Cr, 9.06% of Ni, 0.05% of N, 0.03% of P, 0.22% of Ti and the rest of Fe; heat treatment status: the mechanical properties of the 321 stainless steel at room temperature are as follows: the tensile strength (ab) is 667 MPa, the yield strength (30.2) is 245 MPa, the elongation is 56.5%, and the hardness is 175 HV.
(2) electrolytic polishing: connecting the 321 austenitic stainless steel plate to an anode
at a distance of 50 mm from a cathode made of an insoluble conducting material (graphite
plate), heating an electrolyte to 60°C, soaking the anode and the cathode in the electrolyte
simultaneously, switching on 5V DC voltage, and then taking out the specimen for rinsing
and drying after soaking for 2 min; the electrolyte comprises the following components (by
volume fraction): 60% of concentrated sulfuric acid (98% pure), 37% of concentrated
phosphoric acid (85% pure) and 3% of distilled water.
(3) aluminizing: the solid powder aluminizing medium consists of an aluminium source,
a filler and a permeation promoter (activator), wherein aluminium powder with the particle
size of 200 meshes is taken as the aluminium source, A12 0 3 and Cr powder as the filler and
powder NH 4 Cl as the permeation promoter, all of which are fully mixed based on 5 wt.% of
Cr, 64 wt.% of Al, 28 wt.% of A1 2 0 3 and 3 wt.% of NH 4 Cl; placing the aluminizing medium
and the specimen into a heat-resistance stainless steel tank, compressing, and sealing with a
refractory mortar for aluminizing: conducting furnace heating, drying for 2 h at 150°C,
holding for 20 min at 400°C at a heating rate of10C/min, and conducting furnace cooling to
room temperature after holding for 15 h at 900°C;
(4) sand-blasting treatment: sand-blasting the specimen aluminized under 0.6 MPa high
pressure nitrogen to remove the loose aluminized coatings and impurities, wherein the
abrasive is A12 0 3 particles with 300 meshes, the sand-blasting time is 5 min, and the
sand-blasting distance is 6 cm.
(5) annealing: placing the aluminized specimen into a vacuum tube furnace, annealing
for 1.5 h under a high pure argon at 1,00 0 °C, and taking out after furnace cooling;
(6) laser shock peening treatment: conducting double-sided laser shock peening for the
annealed austenitic stainless steel, wherein the laser wave length is 1,064 nm, the single pulse
energy is 4 J, the pulse width is 10 ns, the spot diameter is 2.8 mm, the overlap rate is 40%,
the black tape is a protective layer, water is a restraint layer, and the number of laser shocks is
1; the path direction of the laser shock treatment is vertical to the rolling direction of the
stainless-steel plate.
The obtained aluminized coating and the substrate and the layers are bound tightly. The
aluminized coating, from outside to inside, includes an uneven A12 0 3 film with a thickness of
20 m, a Fe-Al compound layer (FeAl, FeAl2 and Fe 3Al) with a thickness of 80~100 m, and
an Al-containing Fe phase diffusion layer with a thickness of 60~70 m and a substrate
sequentially, and internally does not include such brittle phases as Fe 2Al 5 and FeA1 3 . The
surface hardness of the aluminized coating is 600~700 HV, and the strengthening depth is
300~400 m. Embodiment 2:
A preparation method for the modified austenitic stainless steel with excellent
high-temperature creep resistance provided by the present invention, comprising the
following steps:
(1) surface mechanical polishing: polishing a hot-rolled austenitic stainless steel
specimen to remove visible scratches using an abrasive paper with different particle sizes
(80~1,200 meshes), ultrasonically cleaning the specimen in acetone for 10 min to remove the
oil, and then ultrasonically cleaning for 10 min in absolute ethyl alcohol to remove stains, and
finally drying in a drying oven for 30 min at 80°C; wherein the 321 austenitic stainless steel is
a rolled plate, and comprises the following chemical components (by mass fraction): 0.04% of
C, 0.38% of Si, 1.08% of Mn, 17.02% of Cr, 9.06% of Ni, 0.05% of N, 0.03% of P, 0.22% of
Ti and the rest of Fe; the mechanical properties of the 321 stainless steel at room temperature:
the tensile strength (G) is 667 MPa, the yield strength (ao.2) is 245 MPa, the elongation is
56.5%, and the hardness is 175 HV.
(2) electrolytic polishing: connecting the 321 austenitic stainless steel to an anode at a
distance of 50 mm from a cathode made of an insoluble conducting material (graphite plate);
heating the electrolyte to 70°C, and soaking the anode and the cathode in the electrolyte;
switching on 5V DC voltage, socking for 5 min in the electrolyte, and taking out the specimen
for cleaning by rinsing and drying, wherein the electrolyte comprises the following
components (by volume fraction): 70% of concentrated sulfuric acid (98% pure), 26% of
concentrated phosphoric acid (85% pure) and 4% of distilled water.
(3) aluminizing: the solid powder aluminizing medium consists of an aluminium source,
a filler and a permeation promoter (activator), wherein aluminium powder with the particle
size of 200 meshes is taken as the aluminium source, A1 2 0 3 and Cr powder as the filler and
powder NH 4 Cl as the permeation promoter, all of which are fully mixed based on 15 wt.% of
Cr, 44 wt.% of Al, 40 wt.% of A1 2 0 3 and 1 wt.% of NH 4 Cl; placing the aluminizing medium
and the specimen into a heat-resistance stainless steel tank, compressing, and sealing with a
refractory mortar for aluminizing: conducting furnace heating, drying for 2 h at 150°C,
holding for 40 min at 600°C at a heating rate of10C/min, and conducting furnace cooling to
room temperature after holding for 10 h at 1,050°C.
(4) sand-blasting treatment: sand-blasting the specimen aluminized under 0.8 MPa high
pressure nitrogen to remove the loose aluminized coatings and impurities, wherein the
abrasive is A12 0 3 particles with 400 meshes, the sand-blasting time is 10 min, and the
sand-blasting distance is 4 cm.
(5) annealing: placing the aluminized specimen into a vacuum tube furnace, annealing
for 0.5 h under a high pure argon at 1,100°C, and taking out after furnace cooling;
(6) laser shock peening treatment: conducting double-sided laser shock peening for the
annealed austenitic stainless steel, wherein the laser wave length is 1,064 nm, the single pulse
energy is 6 J, the pulse width is 30 ns, the spot diameter is 3 mm, the overlap rate is 70%, the
black tape is a protective layer, water is a restraint layer, and the number of laser shocks is 3.
Fig. 1 is the laser shock peening path of this embodiment, which is vertical to a rolling
direction of the stainless-steel plate.
The obtained aluminized coating and the substrate and the layers are bound tightly. The
aluminized coating, from outside to inside, includes an uneven A12 0 3 film with a thickness of
10 pm, a Fe-Al compound layer (FeAl, FeAl 2 and Fe 3Al) with a thickness of 70~80 m, and
an Al-containing Fe phase diffusion layer with a thickness of 50~60 m and a substrate
sequentially, and internally does not include such brittle phases as Fe 2Al 5 and FeA1 3 . The
surface hardness of the aluminized coating is 700~800 HV, and the strengthening depth is
800~1,400 [m. Embodiment 3:
A preparation method for the modified austenitic stainless steel with excellent
high-temperature creep resistance provided by the present invention, comprising the
following steps:
(1) surface mechanical polishing: polishing a hot-rolled austenitic stainless steel plate
specimen to remove visible scratches using an abrasive paper with different particle sizes
(80~1,200 meshes), ultrasonically cleaning the specimen in acetone for 20 min to remove oil,
and then ultrasonically cleaning for 20 min in absolute ethyl alcohol to remove stains, and
finally drying in a drying oven for 40 min at 80°C; wherein the 321 austenitic stainless steel is
a rolled plate, and comprises the following chemical components (by mass fraction): 0.04% of
C, 0.38% of Si, 1.08% of Mn, 17.02% of Cr, 9.06% of Ni, 0.05% of N, 0.03% of P, 0.22% of
Ti and the rest of Fe; the mechanical properties of the 321 stainless steel at room temperature:
the tensile strength (ab) is 667 MPa, the yield strength (ao.2) is 245 MPa, the elongation is
56.5%, and the hardness is 175 HV.
(2) electrolytic polishing: connecting the 321 austenitic stainless steel to an anode at a
distance of 50 mm from a cathode made of an insoluble conducting material (graphite plate),
heating the electrolyte to 80°C, soaking the anode and the cathode in the electrolyte
simultaneously, switching on 5V DC voltage, and then taking out the specimen for rinsing
and drying after soaking for 3 min; the electrolyte comprises the following components (by
volume fraction): 80% of concentrated sulfuric acid (98% pure), 15% of concentrated
phosphoric acid (85% pure) and 5% of distilled water.
(3) aluminizing: the solid powder aluminizing medium consists of an aluminium source,
a filler and a permeation promoter (activator), wherein aluminium powder with the particle
size of 200 meshes is taken as the aluminium source, A1 2 0 3 and Cr powder as the filler and
powder NH 4 Cl as the permeation promoter, all of which are fully mixed based on 10 wt.% of
Cr, 58 wt.% of Al, 30 wt.% of A1 2 0 3 and 2 wt.% of NH 4 Cl; placing the aluminizing medium
and the specimen into a heat-resistance stainless steel tank, compressing, and sealing with a
refractory mortar for aluminizing: conducting furnace heating, drying for 2 h at 150°C,
holding for 30 min at 500°C at a heating rate of10C/min, and conducting furnace cooling to
room temperature after holding for 12 h at 950°C.
(4) sand-blasting treatment: sand-blasting the specimen aluminized under 0.9 MPa high
pressure nitrogen to remove the loose aluminized coatings and impurities, wherein the
abrasive is A12 0 3 particles with 500 meshes, the sand-blasting time is 5 min, and the
sand-blasting distance is 2 cm.
(5) annealing: placing the aluminized specimen into a vacuum tube furnace, annealing
for 1 h under a high pure argon at 1,050°C, and taking out after furnace cooling;
(6) laser shock peening: conducting double-sided laser shock peening treatment for the annealed austenitic stainless steel with a pulse high-energy laser device, wherein the laser wave length is 1,064 nm, the single pulse energy is 7 J, the pulse width is 20 ns, the spot diameter is 2.6 mm, the overlap rate is 50%, the black tape is a protective layer, water is a restraint layer, and the number of laser shocks is 3. Fig. 1 is the laser shock peening path of this embodiment, which is vertical to a rolling direction of the stainless-steel plate. The results of XRD analysis for the aluminized coatings obtained in this embodiment are shown in Fig. 2, namely, the phase components of the aluminized coating mainly comprise FeAl, FeAl 2 and Fe 3Al, and do not comprise brittle phases such as Fe 2Al 5 and FeA 3
. The results of SEM analysis for the aluminized coating obtained in this embodiment are shown in Fig. 3, namely, the aluminized coating and the substrate and the layers are bound tightly with obvious and regular boundaries and no cracks, which indicates that the aluminized coating and the substrate have been bound metallurgically, as shown in Fig. 3(a), points A, B, C and D are taken from outside to inside in the aluminized coating depth direction, their EDS diagram is shown in Figs. 3(b), 3(c), 3(d) and 3(e) (namely, in Fig. 3, (a) is the section appearance; (b) is the EDS energy spectrum corresponding to the point A; (c) is the EDS energy spectrum corresponding to the point B; (d) is the EDS energy spectrum corresponding to the point C; (e) is the EDS energy spectrum corresponding to the point D), wherein the content of Al element decreases gradually, while the content of Fe element increases gradually. The aluminized coating includes, from outside to inside, an uneven A1 2 0 3 film with a thickness of 10 m, a Fe-Al compound (FeAl, FeAl 2 and Fe 3Al) with a thickness of 50~60 pm, and an Al-containing Fe phase diffusion layer with a thickness of 40~50 m and a substrate sequentially. Fig. 4 shows that the microhardness obtained in this embodiment changes in the aluminized coating depth direction, the surface microhardness thereof is 1,390 HV, which is as 7.95 times as the hardness (175 HV) of the 321 stainless steel before being modified, and the strengthening depth is 1,600[tm. Fig. 5 is a high temperature creep curve diagram of comparing the modified 321 austenitic stainless steel obtained in this embodiment with the unmodified 321 austenitic stainless steel under a creep load of 620°C/210 MPa and in the molten Al-Si alloy environment under a creep load of 620°C/210 MPa. As can be seen from Fig. 5, the 321 stainless steel has a high temperature creep rupture time of 105 h at 620°C and 210 MPa, and a steady-state creep rate of 1.3285X 10-7; under the same creep load (210 MPa), the molten
Al-Si alloy will reduce the creep resistance of 321 stainless steel, the creep rupture time is 73
h corresponding to the molten Al-Si environment, and the steady-state creep rate is 2.7143 X
10-7. For the modified 321 austenitic stainless steel obtained in this embodiment in the molten
Al-Si alloy environment, the creep rupture time is 124 h, the steady-state creep rate is 6.0575
X 10-1; compared with the 321 stainless steel, the creep resistance can be improved by one
order of magnitude. Meanwhile, the influence of the molten Al alloy environment can be
ignored in comparison with the ordinary high-temperature creep resistance (the creep rupture
time is 128 h) of the modified 321 austenitic stainless steel obtained in this embodiment.
The above examples are only preferred embodiments of the present invention and not
used to limit the present invention. Any person skilled in the art, without departing from the
scope of the technical solution of the present invention, is capable of taking advantage of the
above-described technical content to make a plurality of possible variations and modifications
of the technical solution, or equivalent embodiments with equivalent changes. Therefore, all
the contents without departing from the technical solution of the present invention, based on
any simple modification, equivalent variations and modifications made by the technical spirit
of the present invention for the above embodiments, would be incorporated in the protection
range of the technical solution of the present invention.
1. A modified austenitic stainless steel with the excellent high-temperature creep
resistance, characterized in that the modified austenitic stainless steel comprising an austenitic
stainless steel substrate and aluminized coating, wherein the aluminized coating, from inside
to outside, comprising an Al-containing Fe phase diffusion layer with a thickness of 40~80
p m, a Fe-Al compound layer with a thickness of 50-100 P mandanA12 0 3 filmwitha
thickness of 10~20 p m;
the Fe-Al compound layer is non-brittle intermetallic compounds of Fe and Al; the
non-brittle intermetallic compound comprises FeAl, FeAl 2 and Fe 3Al;
the surface hardness of the aluminized coating is 625~1,390 HV, and the strengthening
depth is 300~1,600 p m. 2. The modified austenitic stainless steel with the excellent high-temperature creep
resistance as recited in claim 1, characterized in that, the austenitic stainless steel substrate is
321 austenitic stainless steel.
3. A preparation method for the modified austenitic stainless steel with the excellent
high-temperature creep resistance, characterized in that, comprising the following steps:
Si. electrolytic polishing: electrolytically polishing an austenitic stainless steel plate by
taking the austenitic stainless steel plate as an anode and an insoluble conducting material as a
cathode;
S2. aluminizing: drying the austenitic stainless steel after being electrolytically polished,
aluminizing using a solid powder aluminizing medium, wherein the aluminizing conditions
include: first holding for 20~40 min at 400~600°C, and then conducting furnace cooling to
room temperature after holding for 10~15 h at 900~1,050°C;
the solid powder aluminizing medium is a uniform mixture of the following
components: an aluminium powder with a particle size of 200 meshes, a filler consisting of an
A12 0 3 and a Cr powder and a powder NH 4 Cl as a permeation promoter;
S3. sand-blasting treatment: conducting sand-blasting for the specimen aluminized under
0.6~0.9 MPa high pressure nitrogen;
S4. annealing: annealing the specimen after being subject to sand-blasting treatment in
an argon atmosphere at 1,000~1,100°C, and taking out the specimen after furnace cooling; and S5. laser shock peening: conducting laser shock treatment for the specimen after being annealed, wherein the single pulse energy of the laser shock is 4-7 J, the spot diameter is 2.6~3 mm; the number of laser shocks is 1~3; and obtaining the modified austenitic stainless steel after the laser shock peening treatment. 4. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance as recited in claim 3, characterized in that, in the step S2, in the solid powder aluminizing medium, by mass ratio, the aluminium powder is 42~74%, the
A12 0 3 powder is 20~40%, the Cr powder is 5~15%, and the NH 4 C is 1~3%.
5. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance as recited in claim 3, characterized in that, in the step S4, the annealing time is 0.5~3 h. 6. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance as recited in claim 3, characterized in that, in the step S5, a pulse high-energy laser device is applied, a black tape is taken as a protective layer, and water is taken as a restraint layer; the laser has a wave length of 1,064 nm, a pulse width of 10~30 ns, and an overlap rate of 40~70%; the laser shock treatment is a double-sided laser shock treatment; the path direction of the laser shock treatment is vertical to the rolling direction of the stainless steel plate. 7. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance as recited in any claim of claims 3 to 6, characterized in that, in the step S3, the sand-blasting abrasive is A1 2 0 3 particles with 300~500 meshes, and; the sand-blasting time is 5~20 min, and the sand-blasting distance is 2~6 cm. 8. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance as recited in any claim of claims 3 to 6, characterized in that, in the step S, the electrolyte comprises concentrated sulfuric acid with a volume fraction of 60~80%, concentrated phosphoric acid with a volume fraction of 15~37% and distilled water with a volume fraction of 3~5%; the electrolytic DC voltage is 5-6 V, the temperature of the electrolyte is 60-80°C, and the electrolytic polishing time is 2~5 min. 9. The preparation method for the modified austenitic stainless steel with the excellent high-temperature creep resistance as recited in any claim of claims 3 to 6, prior to the step Sl, further comprising a step of conducting surface mechanical polishing treatment for the austenitic stainless steel; the specific steps of the surface mechanical polishing include: grinding to remove visible scratches using an abrasive paper with the particle size varying from 80 to 1,200 meshes, ultrasonically cleaning for 5~20 min in acetone to remove oil, and then ultrasonically cleaning for 5~20 min in absolute ethyl alcohol to remove stains, and finally drying in a drying oven for 20~40 min at 80°C.
1/4
Fig. 2 Fig. 1
2/4
Fig. 3
3/4
Fig. 4
4/4
Fig. 5
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| PCT/CN2019/126131 WO2020147490A1 (en) | 2019-01-17 | 2019-12-18 | Modified austenitic stainless steel having good high-temperature creep resistance performance and preparation method therefor |
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| CN112760591B (en) * | 2020-12-22 | 2023-06-23 | 浦夕特种合金(上海)有限公司 | High-corrosion-resistance stainless steel and preparation method thereof |
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