CN109735798B - Modified austenitic stainless steel with excellent high-temperature creep resistance and preparation method thereof - Google Patents
Modified austenitic stainless steel with excellent high-temperature creep resistance and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a modified austenitic stainless steel with excellent high-temperature creep resistance and a preparation method thereof, wherein the modified steel comprises a steel substrate and a permeable layer, and the permeable layer comprises a 40-80 mu m Fe phase diffusion layer containing Al, a 50-100 mu m Fe-Al compound layer and 10-20 mu m Al from inside to outside2O3A film. The preparation method comprises the following steps: (1) electrolytic polishing; (2) aluminizing: respectively treating at 400-600 ℃ and 900-1050 ℃ and cooling in a furnace; (3) sand blasting: under the nitrogen of 0.6-0.9 MPa; (4) annealing: annealing at 1000-1100 ℃, and furnace cooling; (5) laser shock peening: the single pulse energy is 4-7J, the diameter of a light spot is 2.6-3 mm, and the times are 1-3. The modified steel has excellent creep resistance and corrosion resistance under the condition of melting aluminum-silicon alloy, has no brittle phase in a seeping layer, and has strong bonding force with a matrix, good stripping resistance, toughness and strength.
Description
Technical Field
The invention relates to the technical field of heat exchange tube materials, in particular to modified austenitic stainless steel with excellent high-temperature creep resistance and a preparation method thereof.
Background
Solar thermal Power generation (also called focused Solar thermal Power generation, CSP) has the advantages of stable, continuous and controllable Power output and realization of complementation with photovoltaic Power and wind Power, and is widely regarded as a representative clean energy source in energy structure optimization. The heat storage system is a main link of the CSP power station. At present, the heat storage medium of the commercial CSP power station mainly adopts water vapor, molten salt and heat conduction oil, and because of the characteristics of low heat storage capacity of the water vapor, low heat conductivity coefficient of the molten salt, easy decomposition at high temperature, easy solid-liquid delamination, easy decomposition of the heat conduction oil at high temperature (above 400 ℃), and the like, the heat storage system has the defects of low heat conduction efficiency, poor thermal stability, large supercooling degree and the like, the power generation cost is high, and the development of solar thermal power generation is limited. The latent heat of the aluminum-silicon alloy at 1079 ℃ can reach 960J/g, the heat conductivity coefficient of the aluminum-silicon alloy is more than 2 times of that of salt, after 720 times of melting-solidification circulation at the melting point of 575 ℃, the phase change latent heat is reduced from 505kJ/kg to 452kJ/kg, the reduction amplitude is only 10.5 percent, the phase change temperature basically keeps stable, the aluminum-silicon alloy has the characteristic of high oxidation resistance (after being oxidized at high temperature for hundreds of hours, the oxidation rate is less than 0.01 percent), and the aluminum-silicon alloy is considered as a new generation of heat storage medium substitute material.
However, in practical application, the working conditions and the application environment of the solar thermal power generation heat exchange pipe are extremely severe, constant high stress load and 495-620 ℃ temperature fluctuation need to be borne, the pipe is corroded by the heat storage medium molten aluminum-silicon alloy, and the pipe is corroded, deformed and damaged by creep deformation, so that the service life of a thermal power generation system is shortened. Therefore, the problem of the CSP research and development which needs to be solved urgently is to improve the high-temperature creep resistance of the molten aluminum-silicon alloy of the heat exchange tube material. At present, the method for relieving the corrosion of the molten aluminum-silicon alloy is to aluminize on austenitic stainless steel which is a heat exchange tube material. Aluminizing is now widely used in industrial production as a mature chemical heat treatment process. However, in the common aluminizing process, the composition of the surface phase of the aluminized coating is not easy to control, a brittle phase is easily generated, the thickness of the aluminized coating is often too thin and loose, the aluminized coating is not tightly combined with a matrix and is easy to peel off, the surface strengthening effect is affected, or the strength and the toughness of the material are reduced in the processing process. Therefore, the aluminized steel prepared by the existing aluminizing process has obvious defects in mechanical property, such as: due to the low load bearing capacity of the aluminized layer, insufficient toughness and strength of the material, micropores or microcracks in the aluminized layer are easy to nucleate and rapidly expand on the surface, resulting in aluminized samples exhibiting higher creep deformation rate and shorter creep rupture life.
The laser shock peening is an advanced surface enhancement technology, can refine grains of a surface layer material, improve dislocation density, introduce higher residual compressive stress, and effectively inhibit crack initiation and propagation so as to improve the mechanical property of the material. However, the material treated by both aluminizing and laser impact has the problems that the surface roughness is increased, the coating is easy to peel off, the generated aluminized layer is easy to crack under high-temperature load, and the service life of the workpiece is shortened. For example, patent application No. 201310282671.7 discloses a method for combined treatment of aluminizing and laser shock, which comprises the steps of pre-cleaning, annealing at 550-780 ℃ for 2-3 h, shot blasting, aluminizing at 500-600 ℃ for 4-6 h, post-cleaning and finally laser shock, wherein the aluminized layer generated by the process mainly comprises Fe2Al5The brittle phase is the main phase, the problem of the brittleness of the infiltrated layer is not solved, the coating is easy to peel off in the laser shock process, and the bonding force between the infiltrated layer and the matrix is poor, so that the residual compressive stress introduced by the laser shock strengthening at high temperature is greatly released, and the strengthening effect of the fretting fatigue resistance is poor.
The document 1Cr11NiWMoV steel laser shock peening aluminizing process research (Chinese laser, 2011, 38 (7), 126-130) discloses a method for laser shock peening first and then aluminizing for 12 hours at 510 ℃, the aluminizing temperature in the process is low, the release of residual compressive stress caused by laser shock peening can be effectively avoided, the aluminizing thickness is not influenced, but the main component of an infiltrated layer is FeAl3And after the brittle phase is loaded at high temperature, cracks are easy to nucleate at a diffusion layer, and the residual compressive stress is greatly released, so that the high-temperature mechanical property enhancing effect is poor. The 20111006570.2 patent discloses a laser shock, aluminizing, and laser weldingA method of impacting. The aluminized layer obtained by the method is easy to fall off in the laser impact process, the aluminized thickness is affected, the process is complicated, the treatment period is long, and the production cost is high.
The solar thermal power generation heat exchange tube using the aluminum-silicon alloy as the heat storage medium requires higher high-temperature creep resistance at high temperature (620 ℃) in the use environment of melting the aluminum-silicon alloy. The patent document No. 201310282671.7 can introduce compressive residual stress on the surface of aluminized layer to provide surface strength, but the obtained infiltrated layer has weak bonding force and the infiltrated layer contains Fe2Al5Brittle phase, which is greatly released along with compression residual stress at high temperature, has poor high-temperature strengthening effect and can not meet the long-term operation requirement of the heat exchange tube.
In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is to provide a new process for joint treatment of aluminizing and laser shock, which can obtain modified austenite with uniform structure, no brittle phase, strong bonding force of the aluminized layer and toughened surface-strengthened matrix, and can ensure excellent high-temperature creep resistance of the heat exchange tube.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides modified austenitic stainless steel with excellent creep resistance and corrosion resistance under the condition of melting aluminum-silicon alloy, non-brittle phase of a seeping layer component, strong binding force between the seeping layer and a matrix, good spalling resistance and good toughness and strength, and also provides a method for preparing the modified austenitic stainless steel with simple process, strong binding force between the seeping layer and the matrix, good spalling resistance, no brittle phase, excellent high-temperature creep resistance and corrosion resistance under the condition of melting aluminum-silicon alloy, and good toughness and strength.
In order to solve the technical problems, the invention adopts the technical scheme that:
the modified austenitic stainless steel with excellent high-temperature creep resistance comprises an austenitic stainless steel matrix and a permeable layer, wherein the permeable layer comprises an Al-containing Fe phase diffusion layer with the thickness of 40-80 mu m, an Fe-Al compound layer with the thickness of 50-100 mu m and a layer with the thickness of 1 from inside to outside0 to 20 μm of Al2O3A film.
The modified austenitic stainless steel excellent in high-temperature creep resistance as described above, preferably, the Fe — Al compound layer is a non-brittle intermetallic compound of Fe and Al; the non-brittle intermetallic compound comprises FeAl and FeAl2And Fe3Al。
The modified austenitic stainless steel with excellent high-temperature creep resistance is preferably 321 austenitic stainless steel; the surface hardness of the seeping layer is 625-1390 HV, and the strengthening action depth is 300-1600 mu m.
As a general inventive concept, there is also provided a method of manufacturing a modified austenitic stainless steel excellent in high temperature creep resistance, comprising the steps of:
s1, electrolytic polishing: carrying out electrolytic polishing treatment on the austenitic stainless steel plate by taking the austenitic stainless steel plate as an anode and taking an insoluble conductive material as a cathode;
s2, aluminizing: drying the austenitic stainless steel after electrolytic polishing treatment, and then aluminizing by adopting a solid powder penetrating agent, wherein the aluminizing conditions are as follows: preserving heat for 20-40 min at 400-600 ℃, preserving heat for 10-15 h at 900-1050 ℃, and cooling to room temperature along with a furnace;
s3, sand blasting: sand blasting is carried out on the aluminized sample under high-pressure nitrogen of 0.6-0.9 MPa;
s4, annealing: annealing the sample subjected to sand blasting treatment in an argon atmosphere at 1000-1100 ℃, cooling along with a furnace, and taking out the sample;
s5, laser shock peening: and carrying out laser shock treatment on the annealed sample, wherein the single pulse energy of the laser shock is 4-7J, the diameter of a light spot is 2.6-3 mm, the laser shock frequency is 1-3 times, and carrying out laser shock strengthening treatment to obtain the modified austenitic stainless steel.
In the above method for preparing a modified austenitic stainless steel having excellent creep resistance at high temperature, preferably, in step S2, the solid powder infiltrant comprises a homogeneous mixture of: aluminum powder with particle size of 200 meshes, Al2O3And a filler comprising Cr powder and its powderNH4The aluminum powder accounts for 42-74% of the solid powder penetrant according to mass ratio, and the Al is used as the penetrant2O320-40% of powder, 5-15% of Cr powder and NH4Cl accounts for 1-3%.
In the above method for manufacturing a modified austenitic stainless steel having excellent high-temperature creep resistance, in step S4, the annealing time is preferably 0.5 to 3 hours.
In the above method for preparing a modified austenitic stainless steel with excellent high-temperature creep resistance, preferably, in step S5, a pulsed high-energy laser is used, a black tape is used as a protective layer, and water is used as a constraint layer; the wavelength of the laser is 1064nm, the pulse width is 10-30 ns, and the lap joint rate is 40-70%; the laser shock treatment is double-sided laser shock treatment; the path direction of the laser shock treatment is vertical to the rolling direction of the stainless steel plate.
In the above method for producing a modified austenitic stainless steel having excellent high-temperature creep resistance, in step S3, the abrasive material for blasting is preferably 300-500 mesh Al2O3Particles; the sand blasting time is 5-20 min, and the sand blasting distance is 2-6 cm.
In the above preparation method of the modified austenitic stainless steel with excellent high-temperature creep resistance, preferably, in the step S1, the electrolyte includes 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 direct current voltage of electrolysis is 5-6V, the temperature of the electrolyte is 60-80 ℃, and the time of electrolytic polishing is 2-5 min.
The above method for producing a modified austenitic stainless steel having excellent high-temperature creep resistance preferably further comprises, before step S1, the step of subjecting the austenitic stainless steel to a surface mechanical polishing treatment; the surface mechanical polishing specifically comprises: sanding with sand paper with the granularity of 80-1200 meshes until no obvious scratch is visible to naked eyes, then cleaning with acetone in ultrasonic waves for 5-20 min, removing oil, ultrasonically cleaning with absolute ethyl alcohol for 5-20 min, removing stains, and finally drying in a drying oven at 80 ℃ for 20-40 min.
Compared with the prior art, the invention has the advantages that:
1. the modified austenitic stainless steel has excellent creep resistance under the conditions of molten aluminum-silicon alloy and high-temperature stress due to the excellent tissue structure, and has high material strength and toughness, and the modified austenitic stainless steel sequentially comprises an Al-containing Fe phase diffusion layer with the thickness of 40-80 mu m, an Fe-Al compound layer with the thickness of 50-100 mu m and Al with the thickness of 10-20 mu m from inside to outside of the surface of a matrix2O3The composition of the tissue structure of the film is that the infiltrated layer does not contain a brittle phase, the tissue is uniform, the thickness is controllable, the components between the infiltrated layer and the infiltrated layer are in gradient smooth transition, the interface stress and the tissue defect between the matrix and the infiltrated layer are obviously reduced, the binding force between the matrix and the infiltrated layer is effectively improved, the infiltrated layer is inhibited from falling off, the crack initiation and expansion is inhibited, the creep resistance of the 321 austenitic stainless steel under the conditions of molten aluminum-silicon alloy and high-temperature stress is effectively improved, the working requirement of a solar thermal power generation heat exchange tube based on the molten aluminum-silicon alloy as a heat storage medium can be met, and the film has great academic value and industrial application potential.
2. The diffusion layer of the modified austenitic stainless steel of the present invention does not contain Fe2Al5、FeAl3The equal brittleness phase has strong bearing capacity, good adhesion between the seeping layers and the matrix, and is not easy to peel off.
3. The modified austenitic stainless steel infiltrated layer is tightly combined, has no crack, has obvious and regular boundary, the surface hardness of the infiltrated layer is 625-1390 HV, the strengthening action depth is 300-1600 mu m, and the surface strengthening effect of the material is good.
4. According to the invention, through the specific electrolytic polishing, aluminizing, sand blasting, annealing and laser shock strengthening process steps, 321 stainless steel is treated in a specific sequence and the parameters of aluminizing temperature, sand blasting pressure, annealing temperature, laser shock path, single pulse energy, spot intensity and the like are controlled, so that 10-20 mu m Al is obtained from outside to inside in sequence2O3A thin film, a 50-100 μm thick Fe-Al compound layer (FeAl )2And Fe3Al and an Al (Fe) -containing phase diffusion layer (i.e. an Al-containing Fe phase diffusion layer) having a thickness of 40 to 80 μm,tight combination between the infiltrated layers, no crack, obvious and neat boundary, small stress between each interface, small stress between the substrate and the infiltrated layer interface, good macroscopic morphology of the infiltrated layer surface, fine tissue crystal grains, no crack, uniform tissue, controllable thickness and no Fe2Al5、FeAl3The modified austenitic stainless steel with the equal brittleness phase and the components between the infiltrated layer and the infiltrated layer in gradient smooth transition obviously reduces the interface stress and the tissue defect between the matrix and the infiltrated layer, effectively improves the binding force between the matrix and the infiltrated layer, inhibits the infiltrated layer from falling off, inhibits the crack from growing and expanding, effectively improves the creep resistance of 321 austenitic stainless steel under the conditions of melting aluminum-silicon alloy and high temperature stress, has excellent creep resistance under the conditions of melting aluminum-silicon alloy and high temperature stress, and can improve the matrix strength and the toughness of the austenitic stainless steel.
5. The method can further improve the regulation and control precision of the structure by further controlling the process parameters such as annealing time, penetrating agent composition, laser impact process parameters, sand blasting time, sand blasting distance, electrolytic polishing conditions and the like, thereby further improving the compactness and integrity of the structure, obtaining modified austenite with good surface strengthening and high matrix toughness, and effectively improving the creep resistance, toughness, strength and other properties of the modified austenitic stainless steel under the conditions of melting aluminum-silicon alloy and high-temperature stress.
6. The method of the invention removes impurities and covering substances on the surface of the sample by performing surface mechanical polishing treatment on the austenitic stainless steel sample before electrolytic polishing, improves the cleanliness of the surface of the sample and creates good surface conditions for subsequent aluminizing treatment.
Drawings
FIG. 1 is a schematic diagram of a laser shock peening process performed on an austenitic stainless steel sample according to the present invention.
Figure 2 XRD contrast plots of the modified 321 austenitic stainless steel prepared in example 3 of the present invention and the unmodified 321 austenitic stainless steel.
FIG. 3 is an EDS spectrum analysis chart of the cross-sectional profile and corresponding points of the modified 321 austenitic stainless steel prepared in example 3 of the present invention.
Fig. 4 is a graph showing the change in microhardness of a modified 321 austenitic stainless steel prepared in example 3 of the present invention in the depth direction of a carburized layer.
FIG. 5 is a graph comparing the high temperature creep at 620 deg.C/210 MPa and 620 deg.C/210 MPa in a molten Al-Si alloy environment for a modified 321 austenitic stainless steel prepared in example 3 of the present invention and an unmodified 321 austenitic stainless steel.
Detailed Description
The invention will be described in further detail below with reference to the drawings and specific examples.
The modified austenitic stainless steel with excellent high-temperature creep resistance comprises an austenitic stainless steel matrix, an Al-containing Fe phase diffusion layer with the thickness of 40-80 mu m, an Fe-Al compound layer with the thickness of 50-100 mu m and Al with the thickness of 10-20 mu m from inside to outside2O3A film.
The Fe-Al compound layer is a non-brittle intermetallic compound of Fe and Al, including FeAl and FeAl2And Fe3Al。
The austenitic stainless steel matrix is 321 austenitic stainless steel.
The preparation method of the modified austenitic stainless steel with excellent high-temperature creep resistance comprises the following steps:
(1) and (3) mechanically polishing the surface: polishing austenitic stainless steel plates of hot rolled plates by abrasive paper with different particle sizes (80-1200 #) until no obvious scratch is visible to naked eyes, then cleaning for 5-20 min by adopting acetone in ultrasonic waves, removing oil, cleaning for 5-20 min by using absolute ethyl alcohol ultrasonic waves, removing stains, and finally drying for 20-40 min in a drying oven at 80 ℃; wherein the 321 austenitic stainless steel is a rolled plate, and comprises the chemical components of, by mass, 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 balance of Fe. The mechanical properties of 321 stainless steel at normal temperature are as follows: tensile strength (sigma b) 667MPa, yield strength (sigma 0.2) 245 MPa, elongation 56.5%, hardness 175 HV.
(2) Electrolytic polishing: connect 321 austenite stainless steel at the positive pole, insoluble conductive material (graphite cake) for the negative pole, negative and positive pole interval 50mm, electrolyte heating to 60 ~ 80 ℃ (accessible water bath heating), let in 5 ~ 6V direct current voltage, polish in the electrolysis after 2 ~ 5min, take out austenite stainless steel and wash by water and wash and weather, wherein the composition of electrolyte is as follows: 60-80% by volume of concentrated sulfuric acid (with the purity of 98%), 15-37% by volume of concentrated phosphoric acid (with the purity of 85%) and 3-5% by volume of distilled water.
(3) Aluminizing: the solid powder penetrating agent consists of an aluminum source, a filling agent and a penetration assisting agent (an activating agent), wherein the aluminum source adopts aluminum powder with the granularity of 200 meshes and Al2O3And Cr powder as filler and powdered NH4The permeation assistant agent of Cl is composed of 5-15 wt.% of Cr, 42-74 wt.% of Al and 20-40 wt.% of Al2O3，1～3wt.%NH4Cl was mixed well. Putting the infiltration agent and the austenitic stainless steel plate subjected to electrolytic polishing into a heat-resistant stainless steel material tank, compacting, sealing by using refractory clay, and carrying out aluminizing: heating along with the furnace, drying at 150 ℃ for 2h, then preserving heat at 400-600 ℃ for 20-40 min at the heating rate of 10 ℃/min, preserving heat at 900-1050 ℃ for 10-15 h, and then cooling along with the furnace to room temperature.
(4) Sand blasting treatment: the aluminized austenitic stainless steel plate is put under 0.6-0.9 MPa high-pressure nitrogen for sand blasting, and the abrasive is 300-500 meshes of Al2O3And (3) carrying out particle blasting for 5-20 min, wherein the sand blasting distance is 2-6 cm, and removing loose seepage layers and impurities.
(5) Annealing: and (3) putting the aluminized austenitic stainless steel plate into a vacuum tube furnace, annealing for 0.5-3 h at 1000-1100 ℃ under high-purity argon, and cooling along with the furnace and taking out.
(6) Laser shock peening: and carrying out double-sided laser shock strengthening treatment on the annealed austenitic stainless steel plate, wherein the laser wavelength is 1064nm, the single pulse energy is 4-7J, the pulse width is 10-30 ns, the diameter of a light spot is 2.6-3 mm, the lap joint rate is 40-70%, the black adhesive tape is a protective layer, water is a constraint layer, and the laser shock frequency is 1-3 times (1 time, 2 times or 3 times). Fig. 1 shows a laser shock peening path, which is perpendicular to the rolling direction of a stainless steel sheet.
Enhanced resistance to melting of the inventionThe modified austenitic stainless steel with aluminum-silicon alloy high-temperature creep property and the preparation method thereof have the advantages that after the austenitic stainless steel is aluminized and subjected to laser impact, the surface of an aluminized layer has good macroscopic appearance, the structure crystal grains are fine, and no cracks exist. The infiltration layer is of a multilayer structure and is respectively made of 10-20 mu m of Al with unevenness from outside to inside in sequence2O3A thin film, a 50-100 μm thick Fe-Al compound (FeAl )2And Fe3Al), a 40-80 μm thick Al (Fe) -containing phase diffusion layer and a substrate. And the penetrated layers are tightly combined, have no cracks and have obvious and regular boundaries. The surface hardness of the infiltrated layer is 625-1390 HV, and the strengthening depth is 300-1600 μm. Under the environment of 620 ℃ molten aluminum-silicon alloy, the high-temperature tensile creep rupture time under 210MPa creep load is more than 94h, and the steady-state creep rate is 1.1254 x 10-7Below, compared with 321 steel (creep rupture time 73h, steady state creep rate 2.7143 x 10)-7) The steady-state creep rate is greatly reduced, the high-temperature creep resistance of the molten aluminum-silicon alloy is shown, the working requirement of the solar thermal power generation heat exchange tube based on the molten aluminum-silicon alloy as the heat storage medium is met, and the high-temperature creep resistance heat exchange tube has high academic value and industrial application potential.
Example 1:
the preparation method of the modified austenitic stainless steel with excellent high-temperature creep resistance comprises the following steps:
(1) and (3) mechanically polishing the surface: grinding hot rolled sheet austenitic stainless steel plate samples by abrasive paper with different particle sizes (80-1200 meshes) until no obvious scratch is visible to naked eyes, then cleaning for 5min by adopting acetone in ultrasonic waves, removing oil, cleaning for 5min by using absolute ethyl alcohol in ultrasonic waves, removing stains, and finally drying for 20min in a drying oven at 80 ℃; wherein the 321 austenitic stainless steel is a rolled plate, and comprises the chemical components of, by mass, 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 balance of Fe. Heat treatment state: the mechanical properties of 321 stainless steel at normal temperature are as follows: tensile strength (σ)b) 667MPa, yield strength (. sigma.)0.2) 245 MPa, elongation 56.5% and hardness 175 HV.
(2) Electrolytic polishing: connecting a 321 austenitic stainless steel plate at an anode, using an insoluble conductive material (graphite plate) as a cathode, enabling the distance between the cathode and the anode to be 50mm, heating an electrolyte to 60 ℃, simultaneously enabling the two electrodes to enter the electrolyte, introducing 5V direct-current voltage, soaking for 2min in electrolysis, taking out a sample, flushing, cleaning and drying; the electrolyte consists of 60% by volume concentrated sulfuric acid (purity 98%), 37% by volume concentrated phosphoric acid (purity 85%) and 3% by volume distilled water.
(3) Aluminizing: the solid powder penetrating agent consists of an aluminum source, a filling agent and a penetration assisting agent (an activating agent), wherein the aluminum source adopts aluminum powder with the granularity of 200 meshes and Al2O3And Cr powder as filler and powdered NH4A permeation enhancer of Cl in an amount of 5wt.% Cr, 64wt.% Al, 28wt.% Al2O3，3wt.%NH4Cl was mixed well. Putting the penetrating agent and the sample into a heat-resistant stainless steel material tank, compacting, sealing refractory mortar, and aluminizing: heating with a furnace, drying at 150 deg.C for 2h, maintaining at 400 deg.C for 20min at a heating rate of 10 deg.C/min, maintaining at 900 deg.C for 15h, and cooling with the furnace to room temperature.
(4) Sand blasting treatment: the aluminized sample is put under 0.6MPa high-pressure nitrogen for sand blasting, and the grinding material is 300-mesh Al2O3And (4) carrying out particle blasting for 5min and 6cm, and removing loose seepage layers and impurities.
(5) Annealing: putting the aluminized sample into a vacuum tube furnace, annealing for 1.5h at 1000 ℃ under high-purity argon, and cooling along with the furnace to take out the sample.
(6) Laser shock peening: the aluminized stainless steel is subjected to double-sided laser shock strengthening treatment, the laser wavelength is 1064nm, the single pulse energy is 4J, the pulse width is 10ns, the diameter of a light spot is 2.8mm, the lap joint rate is 40%, the black adhesive tape is a protective layer, water is a constraint layer, and the laser shock frequency is 1 time. The path direction of the laser shock treatment is perpendicular to the rolling direction of the stainless steel plate.
The obtained infiltrated layer is tightly combined with the matrix and the interlayer, and the infiltrated layer is respectively rugged 20 μm thick Al from outside to inside2O3A thin film, a Fe-Al compound layer (FeAl ) having a thickness of 80 to 100 μm2And Fe3Al), a 60 to 70 μm thick Fe phase diffusion layer containing Al, andthe matrix and the infiltrated layer do not contain Fe2Al5、FeAl3And the like brittle phase. The surface hardness of the infiltrated layer is 600-700 HV, and the strengthening depth is 300-400 μm.
Example 2:
the preparation method of the modified austenitic stainless steel with excellent high-temperature creep resistance comprises the following steps:
(1) and (3) mechanically polishing the surface: grinding austenitic stainless steel samples of the hot rolled plate by abrasive paper with different particle sizes (80-1200 meshes) until no obvious scratch is visible to naked eyes, then cleaning for 10min by adopting acetone in ultrasonic waves, removing oil, cleaning for 10min by using absolute ethyl alcohol in ultrasonic waves, removing stains, and finally drying for 30min in a drying oven at 80 ℃; wherein the 321 austenitic stainless steel is a rolled plate, and comprises the chemical components of, by mass, 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 balance of Fe. The mechanical properties of 321 stainless steel at normal temperature are as follows: tensile strength (σ)b) 667MPa, yield strength (. sigma.)0.2) 245 MPa, elongation 56.5% and hardness 175 HV.
2) Electrolytic polishing: connecting 321 austenitic stainless steel at an anode, using an insoluble conductive material (graphite plate) as a cathode, enabling the distance between the cathode and the anode to be 50mm, heating an electrolyte to 70 ℃, simultaneously enabling the two electrodes to enter the electrolyte, introducing 5V direct current voltage, soaking for 5min in electrolysis, taking out a sample, flushing, cleaning and blow-drying, wherein the electrolyte comprises concentrated sulfuric acid with the volume fraction of 70% (with the purity of 98%), concentrated phosphoric acid with the volume fraction of 26% (with the purity of 85%) and distilled water with the volume fraction of 4%.
(3) Aluminizing: the solid powder penetrating agent consists of an aluminum source, a filling agent and a penetration assisting agent (an activating agent), wherein the aluminum source adopts aluminum powder with the granularity of 200 meshes and Al2O3And Cr powder as filler and powdered NH4A permeation enhancer of Cl in an amount of 15wt.% Cr, 44wt.% Al, 40wt.% Al2O3，1wt.%NH4Cl was mixed well. Putting the penetrating agent and the sample into a heat-resistant stainless steel material tank, compacting, sealing refractory mortar, and aluminizing: heating with furnace, drying at 150 deg.C for 2 hr, maintaining at 600 deg.C for 40min at a heating rate of 10 deg.C/min at 10 deg.CKeeping the temperature at 50 ℃ for 10h, and then cooling the mixture to room temperature along with the furnace.
(4) Sand blasting treatment: the aluminized sample is put under 0.8MPa high-pressure nitrogen for sand blasting, and the grinding material is 400-mesh Al2O3And (4) carrying out particle blasting for 10min and 4cm, and removing loose seepage layers and impurities.
(5) Annealing: putting the aluminized sample into a vacuum tube furnace, annealing for 0.5h at 1100 ℃ under high-purity argon, and cooling along with the furnace to take out the sample.
(6) Laser shock peening: the aluminized stainless steel is subjected to double-sided laser shock strengthening treatment, the laser wavelength is 1064nm, the single pulse energy is 6J, the pulse width is 30ns, the diameter of a light spot is 3mm, the lap joint rate is 70%, the black adhesive tape is a protective layer, water is a constraint layer, and the laser shock times are 3 times. Fig. 1 shows the laser shock peening path of the present embodiment, the path direction being perpendicular to the rolling direction of the stainless steel plate.
The obtained infiltrated layer is tightly combined with the matrix and the interlayer, and the infiltrated layer is respectively rugged 10 mu m thick Al from outside to inside in sequence2O3A thin film, a 70-80 μm thick Fe-Al compound layer (FeAl )2And Fe3Al), a 50-60 μm thick Al-containing Fe phase diffusion layer and a matrix, the diffusion layer not containing Fe2Al5、FeAl3And the like brittle phase. The surface hardness of the infiltrated layer is 700-800 HV, and the strengthening depth is 800-1400 μm.
Example 3:
the preparation method of the modified austenitic stainless steel with excellent high-temperature creep resistance comprises the following steps:
(1) and (3) mechanically polishing the surface: grinding austenitic stainless steel samples of the hot rolled plate by abrasive paper with different particle sizes (80-1200 meshes) until no obvious scratch is visible to naked eyes, then cleaning the samples in ultrasonic waves by adopting acetone for 20min, removing oil, cleaning the samples in the ultrasonic waves by absolute ethyl alcohol for 20min, removing stains, and finally drying the samples in a drying oven at 80 ℃ for 40 min; wherein the 321 austenitic stainless steel is a rolled plate, and comprises the chemical components of, by mass, 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 balance of Fe. The mechanical properties of 321 stainless steel at normal temperature are as follows: the tensile strength (. sigma.b) was 667MPa, the yield strength (. sigma.0.2) was 245 MPa, the elongation was 56.5%, and the hardness was 175 HV.
(2) Electrolytic polishing: connecting 321 austenitic stainless steel at an anode, using insoluble conductive materials (graphite plates) as cathodes, enabling the distance between the cathodes and the anodes to be 50mm, heating electrolyte to 80 ℃, simultaneously enabling the two electrodes to enter the electrolyte, introducing 5V direct current voltage, soaking in the electrolyte for 3min, taking out a sample, flushing, cleaning and drying; the electrolyte consists of 80% by volume of concentrated sulfuric acid (purity 98%), 15% by volume of concentrated phosphoric acid (purity 85%) and 5% by volume of distilled water.
(3) Aluminizing: the solid powder penetrating agent consists of an aluminum source, a filling agent and a penetration assisting agent (an activating agent), wherein the aluminum source adopts aluminum powder with the granularity of 200 meshes and Al2O3And Cr powder as filler and powdered NH4A permeation enhancer of Cl in an amount of 10wt.% Cr, 58wt.% Al, 30wt.% Al2O3，2wt.%NH4Cl was mixed well. Putting the penetrating agent and the sample into a heat-resistant stainless steel material tank, compacting, sealing refractory mortar, and aluminizing: heating with a furnace, drying at 150 deg.C for 2h, maintaining at 500 deg.C for 30min at a heating rate of 10 deg.C/min, maintaining at 950 deg.C for 12h, and cooling with the furnace to room temperature.
(4) Sand blasting treatment: the aluminized sample is put under 0.9MPa high-pressure nitrogen for sand blasting, and the grinding material is 500-mesh Al2O3And (4) carrying out particle blasting for 5min and carrying out sand blasting for 2cm, and removing loose seepage layers and impurities.
(5) Annealing: putting the aluminized sample into a vacuum tube furnace, annealing for 1h at 1050 ℃ under high-purity argon, and cooling along with the furnace to take out the sample.
(6) Laser shock peening: the aluminized stainless steel is subjected to double-sided laser strengthening treatment by adopting a pulse high-energy laser, the laser wavelength is 1064nm, the single-pulse energy is 7J, the pulse width is 20ns, the diameter of a light spot is 2.6mm, the lap joint rate is 50%, the black adhesive tape is a protective layer, water is a constraint layer, and the laser impact frequency is 3 times. Fig. 1 shows the laser shock peening path of the present embodiment, the path direction being perpendicular to the rolling direction of the stainless steel plate.
For the present embodimentXRD analysis of the obtained infiltrated layer showed that the infiltrated layer consisted mainly of FeAl and FeAl, as shown in FIG. 22And Fe3Al composition, Fe is not contained in the infiltrated layer2Al5、FeAl3And the like brittle phase.
SEM analysis is carried out on the infiltrated layer prepared in the embodiment, the infiltrated layer and the matrix and the interlayer are tightly combined, no crack is generated, the boundary is obvious and neat, and the metallurgical bonding between the infiltrated layer and the matrix is shown in figure 3, as shown in figure 3 (a), A, B, C, D points are taken from outside to inside along the depth direction of the infiltrated layer, the EDS diagram is sequentially shown in figures 3 (B), 3 (C), 3 (D) and 3 (e) (namely in figure 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, and (e) is the EDS energy spectrum corresponding to the point D, wherein the content of Al element is gradually reduced, and the content of Fe element is gradually increased. The infiltrated layers are respectively uneven 10 mu m thick Al from outside to inside2O3A film, and Fe-Al compounds (including FeAl and FeAl) with a thickness of 50-60 μm2And Fe3Al), an Al-containing Fe phase diffusion layer with a thickness of 40-50 μm, and a substrate.
FIG. 4 shows the change of microhardness with the depth direction of the penetrated layer, the microhardness of the surface of the steel sheet prepared in this example is 1390HV, which is 7.95 times of the hardness (175 HV) of 321 stainless steel before modification, and the strengthening depth is 1600 μm.
FIG. 5 is a graph comparing the high temperature compressive creep curve at 620 deg.C/210 MPa creep load of the modified 321 austenitic stainless steel prepared in this example with that of the unmodified 321 austenitic stainless steel, and the high temperature compressive creep curve at 620 deg.C/210 MPa creep load in molten Al-Si alloy environment, and it can be seen from FIG. 5 that the high temperature creep rupture time at 620 deg.C and 210MPa of the 321 stainless steel is 105h, and the steady state creep rate is 1.3285 × 10-7Under the same creep load (210 MPa), the creep resistance of 321 stainless steel can be reduced by the molten aluminum-silicon alloy, the corresponding creep rupture time under the molten aluminum-silicon environment is 73h, and the steady-state creep rate is 2.7143 × 10-7(ii) a The creep rupture time of the modified 321 austenitic stainless steel prepared in the embodiment in the molten aluminum-silicon alloy environment is 124h, and the steady stateCreep rate 6.0575 × 10-8Compared with 321 steel, the creep resistance is improved by 1 order of magnitude; meanwhile, compared with the common high-temperature creep property (creep rupture time is 128 h) of the modified 321 austenitic stainless steel prepared by the embodiment, the influence of the molten aluminum alloy environment is negligible.
Although the present invention has been described with reference to the preferred embodiments, it is not intended to be limited thereto. Those skilled in the art can make numerous possible variations and modifications to the present invention, or modify equivalent embodiments to equivalent variations, without departing from the scope of the invention, using the teachings disclosed above. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical spirit of the present invention should fall within the protection scope of the technical scheme of the present invention, unless the technical spirit of the present invention departs from the content of the technical scheme of the present invention.
Claims (9)
1. The modified austenitic stainless steel with excellent high-temperature creep resistance is characterized by comprising an austenitic stainless steel matrix and a permeable layer, wherein the permeable layer comprises an Al-containing Fe phase diffusion layer with the thickness of 40-80 mu m, an Fe-Al compound layer with the thickness of 50-100 mu m and Al with the thickness of 10-20 mu m from inside to outside2O3A film; the Fe-Al compound layer is a non-brittle intermetallic compound of Fe and Al; the non-brittle intermetallic compound comprises FeAl and FeAl2And Fe3Al; the surface hardness of the seeping layer is 625-1390 HV, and the strengthening action depth is 300-1600 mu m.
2. The modified austenitic stainless steel having excellent high temperature creep resistance according to claim 1, wherein the austenitic stainless steel matrix is 321 austenitic stainless steel.
3. The preparation method of the modified austenitic stainless steel with excellent high-temperature creep resistance is characterized by comprising the following steps:
s1, electrolytic polishing: carrying out electrolytic polishing treatment on the austenitic stainless steel by taking the austenitic stainless steel as an anode and taking an insoluble conductive material as a cathode;
s2, aluminizing: drying the austenitic stainless steel after electrolytic polishing treatment, and then aluminizing by adopting a solid powder penetrating agent, wherein the aluminizing conditions are as follows: preserving heat for 20-40 min at 400-600 ℃, preserving heat for 10-15 h at 900-1050 ℃, and cooling to room temperature along with a furnace; the solid powder penetrant comprises a uniform mixture of the following components: aluminum powder with particle size of 200 meshes, Al2O3And a filler consisting of Cr powder and powdered NH thereof4A permeation enhancer of Cl;
s3, sand blasting: carrying out sand blasting on the aluminized austenitic stainless steel under high-pressure nitrogen of 0.6-0.9 MPa;
s4, annealing: annealing the austenitic stainless steel subjected to sand blasting treatment in an argon atmosphere at 1000-1100 ℃, cooling along with a furnace, and taking out;
s5, laser shock peening: and (3) carrying out laser shock treatment on the annealed austenitic stainless steel, wherein the single pulse energy of the laser shock is 4-7J, the diameter of a light spot is 2.6-3 mm, the laser shock frequency is 1-3 times, and carrying out laser shock strengthening treatment to obtain the modified austenitic stainless steel.
4. The method of manufacturing a modified austenitic stainless steel having excellent high temperature creep resistance according to claim 3, wherein in the step S2, the aluminum powder accounts for 42 to 74% by mass of the solid powder infiltration agent, and the Al accounts for 42 to 74% by mass of the solid powder infiltration agent2O320-40% of powder, 5-15% of Cr powder and NH4Cl accounts for 1-3%.
5. The method of manufacturing a modified austenitic stainless steel excellent in high temperature creep resistance according to claim 3, wherein the annealing time in the step S4 is 0.5 to 3 hours.
6. The method of manufacturing a modified austenitic stainless steel having excellent high temperature creep resistance according to claim 3, wherein in the step S5, a pulsed high energy laser is used, a black tape is used as a protective layer, and water is used as a constraining layer; the wavelength of the laser is 1064nm, the pulse width is 10-30 ns, and the lap joint rate is 40-70%; the laser shock treatment is 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 method of manufacturing a modified austenitic stainless steel excellent in high temperature creep resistance according to any of claims 3 to 6, wherein the grit blasted in the step S3 is Al of 300 to 500 mesh2O3Particles; the sand blasting time is 5-20 min, and the sand blasting distance is 2-6 cm.
8. The method of manufacturing a modified austenitic stainless steel excellent in high temperature creep resistance according to any of claims 3 to 6, wherein the electrolyte solution in the step S1 comprises concentrated sulfuric acid with a volume fraction of 60 to 80%, concentrated phosphoric acid with a volume fraction of 15 to 37%, and distilled water with a volume fraction of 3 to 5%; the direct current voltage of electrolysis is 5-6V, the temperature of the electrolyte is 60-80 ℃, and the time of electrolytic polishing is 2-5 min.
9. The method of producing a modified austenitic stainless steel excellent in high temperature creep resistance according to any of claims 3 to 6, further comprising a step of subjecting the austenitic stainless steel to surface mechanical polishing treatment before the step S1; the surface mechanical polishing specifically comprises: sanding with sand paper with the granularity of 80-1200 meshes until no obvious scratch is visible to naked eyes, then cleaning with acetone in ultrasonic waves for 5-20 min, removing oil, ultrasonically cleaning with absolute ethyl alcohol for 5-20 min, removing stains, and finally drying at 80 ℃ for 20-40 min.
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| WO2007054265A2 (en) * | 2005-11-08 | 2007-05-18 | Man Turbo Ag | Heat-insulating protective layer for a component located within the hot gas zone of a gas turbine |
| CN101698930A (en) * | 2009-10-09 | 2010-04-28 | 江苏大学 | Reinforcement method for extending fretting fatigue life of material at high temperature |
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