CN109735798A - The excellent modification austenitic stainless steel and preparation method thereof of high temperature creep resistance - Google Patents
The excellent modification austenitic stainless steel and preparation method thereof of high temperature creep resistance Download PDFInfo
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- CN109735798A CN109735798A CN201910044334.1A CN201910044334A CN109735798A CN 109735798 A CN109735798 A CN 109735798A CN 201910044334 A CN201910044334 A CN 201910044334A CN 109735798 A CN109735798 A CN 109735798A
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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
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- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
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- 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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- 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
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- 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
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Abstract
The invention discloses the excellent modification austenitic stainless steel of high temperature creep resistance and preparation methods, the modified steel includes steel matrix and infiltration layer, and infiltration layer includes 40~80 μm of Fe phase diffusion layer, 50~100 μm of Fe-Al compound layer and 10~20 μm of the Al containing Al from the inside to the outside2O3Film.Preparation method includes: (1) electrobrightening；(2) it aluminising: is handled respectively at 400~600 DEG C and 900 DEG C~1050 DEG C, furnace is cold；(3) it sandblasting: is carried out under 0.6~0.9MPa nitrogen；(4) it anneals: annealing at 1000~1100 DEG C, furnace is cold；(5) laser impact intensified: 4~7J of single pulse energy, 2.6~3mm of spot diameter, number 1~3 time.Modified steel of the invention under melting aluminum alloy condition creep-resistant property and corrosion resistance is excellent, infiltration layer without brittlement phase, with basal body binding force is strong, antistrip performance and toughness and intensity are good.
Description
Technical field
The present invention relates to heat exchange tube material technical field more particularly to a kind of modification austenites that high temperature creep resistance is excellent
Stainless steel and preparation method thereof.
Background technique
Solar thermal energy power generation (also referred to as focus type solar energy generate electricity, Concentrating Solar Power, CSP) because
It is exported with electric power stable, continuous, controllable out and can realize the advantage with photovoltaic, wind-electricity complementary, in energy structure optimizing
The middle representative as clean energy resource is widely paid attention to.Heat reservoir is the key link in the power station CSP.Commercialization at present
The power station CSP heat-storage medium mainly uses vapor, fuse salt and conduction oil, since vapor heat storage capacity is low, fuse salt
The features such as thermal coefficient low and high temperature is easily decomposed and solid-liquid layering, and heat-conductive-oil high-temperature (at 400 DEG C or more) easily decomposes, therefore heat accumulation
System there are heat transfer efficiencies it is low, thermal stability is poor, degree of supercooling is big the defects of, cause cost of electricity-generating high, limit solar heat hair
The development of electricity.For alusil alloy in 1079 DEG C of latent heat up to 960J/g, thermal coefficient is the 2 times or more of salt, is 575 in fusing point
At DEG C after 720 melting-solidifications recycle, latent heat of phase change drops to 452kJ/kg by 505kJ/kg, and the range of decrease only has 10.5%,
And phase transition temperature kept stable, have the characteristics that antioxygenic property it is high (after several hundred hours high-temperature oxydations, oxygenation efficiency
Less than 0.01%), it is considered to be heat-storage medium a new generation alternative materials.
But in practical applications, the operating condition and application environment of solar energy thermal-power-generating heat exchange pipe fitting are extremely severe, need
Constant high stress load and 495~620 DEG C of temperature fluctuation are born, by heat-storage medium melting aluminum alloy corrosion,
Corrosion deformation of creep damage occurs, and then shortens the service life of heat generating system.Therefore the resist melt of heat exchange tube material is improved
Alusil alloy high temperature creep property is CSP research and development urgent problem to be solved.At present alleviate melting aluminum alloy corrosion method be
Aluminising is carried out on heat exchange tube material austenitic stainless steel.Aluminising has been answered extensively as a kind of chemical heat treatment process of maturation
For industrial production.But calorized coating Surface Phases composition is not easy to control in common alumetizing process, is easy to produce brittlement phase, seeps
Thickness degree is often excessively thin, loose, not close, easy in conjunction with matrix to be peeled off, and material in surface peening effect or treatment process is influenced
Intensity and toughness reduce.As it can be seen that using existing alumetizing process preparation alumetized steel there is also significantly not in mechanical property
Foot, such as: since the load of aluminized coating is lower, toughness of material and intensity are inadequate, micropore or micro-crack Yi Biao in infiltration layer
Face forming core and Quick Extended, cause aluminising sample to show higher creep strain rate and shorter life-span of creep rupture.
Laser impact intensified is a kind of advanced surface enhancement techniques, enables to skin-material crystal grain refinement, dislocation is close
Degree improves, and introduces higher residual compressive stress, can inhibit crack initiation and propagation, effectively to improve the mechanical property of material
Energy.However, aluminising and laser-impact be jointly processed by after material there are surface roughness increase, coating easily peels off, the infiltration of generation
The problem of aluminium layer is easy cracking under high temperature load, shortens the workpiece service life.For example, number of patent application is 201310282671.7
Patent discloses the method for a kind of aluminising and laser-impact combined processing, and technical process is preceding cleaning, in 550~780 DEG C of annealing 2
~3h, shot-peening, in 500~600 DEG C of 4~6h of aluminising, rear cleaning, last laser-impact, the infiltration layer ingredient of the Process Production is main
With Fe2Al5Based on brittlement phase, Brittleness is not solved the problems, such as, laser-impact process floating coat is easy-peel to be fallen, and infiltration layer and matrix
Binding force is poor, so that the residual compressive stress of laser impact intensified introducing substantially discharges under high temperature, fretting fatigue drag reinforcing effect
Difference.
Document " alumetizing process research after 1Cr11NiWMoV steel is laser impact intensified " (Chinese laser, 2011,38(7), 126
~130) disclose a kind of elder generation it is laser impact intensified, after at 510 DEG C aluminising 12h method, the technique aluminising temperature is relatively low,
It can effectively avoid the laser impact intensified release for introducing residual compressive stress, do not influence aluminising thickness, but the main component of infiltration layer
For FeAl3Brittlement phase, after loading at high temperature, crackle is easy at infiltration layer forming core and will lead to residual compressive stress substantially to discharge,
Cause mechanical behavior under high temperature reinforcing effect bad.Application No. is 20111006570.2 patents to disclose a kind of first laser-impact,
Aluminising again, the method for last laser-impact.This method obtain aluminized coating be easy to fall off during laser-impact, aluminising thickness by
To influence, technique is cumbersome, long processing period, high production cost.
(620 DEG C) are in melting aluminum under solar energy thermal-power-generating heat exchanger tube requirement high temperature using alusil alloy as heat-storage medium
Properties of High Temperature Creep with higher under the use environment of alloy.Though application No. is 201310282671.7 patent document energy
Compressive residual stress is introduced in aluminising layer surface, provides surface strength, but AdhesionStrength obtained is not strong, infiltration layer ingredient contains
Fe2Al5Brittlement phase, with the substantially release of compressive residual stress under high temperature, High-Temperature Strengthening effect is poor, be not able to satisfy heat exchanger tube it is long when
Service requirement.
In view of the drawbacks described above of the above technology, technical problem to be solved by the invention is to provide a kind of aluminising and laser
The new process being jointly processed by is impacted, which can get even tissue, without brittlement phase, and AdhesionStrength is strong, surface strengthened substrate
The modification austenite of toughening, it is ensured that heat exchanger tube high temperature resistant croop property is excellent.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, provide a kind of item in melting aluminum alloy
Creep-resistant property and corrosion resistance is excellent, strong, the anti-stripping without the binding force between brittlement phase, infiltration layer and matrix of infiltration layer ingredient under part
Fall that performance is good, and toughness and the good modification austenitic stainless steel of intensity, additionally provide a kind of simple process, can prepare infiltration layer with
Basal body binding force is strong, antistrip performance is good, without brittlement phase, under conditions of melting aluminum alloy Properties of High Temperature Creep and anti-
Corrosive nature is excellent, and the method for toughness and the good modification austenitic stainless steel of intensity.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
The excellent modification austenitic stainless steel of high temperature creep resistance, the modified austenitic stainless steel include austenite stainless base steel
Body and infiltration layer, the infiltration layer include from the inside to the outside with a thickness of 40~80 μm the Fe phase diffusion layer containing Al, with a thickness of 50~100 μ
The Fe-Al compound layer of m and with a thickness of 10~20 μm of Al2O3Film.
The excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the Fe-Al compound layer is Fe
With the non-brittle intermetallic compound of Al；The non-brittle intermetallic compound includes FeAl, FeAl2And Fe3Al。
The excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the austenite stainless steel matrix
For 321 austenitic stainless steels；The surface hardness of the infiltration layer is 625~1390HV, and invigoration effect depth is 300~1600 μm.
The inventive concept total as one also provides a kind of system of modification austenitic stainless steel that high temperature creep resistance is excellent
Preparation Method includes the following steps:
S1, electrobrightening: using austenite stainless steel plate as anode, using insoluble conductive material as cathode, to austenitic stainless steel
Plate carries out electrobrightening processing；
S2, aluminising: being dried the austenitic stainless steel handled through electrobrightening, then is seeped using solid powder penetration enhancer
Aluminium, the condition of the aluminising are as follows: prior to 400~600 DEG C 20~40min of heat preservation, then at 900 DEG C~1050 DEG C 10~15h of heat preservation
After cool to room temperature with the furnace；
S3, blasting treatment: the sample after aluminising is subjected to sandblasting under the high pressure nitrogen of 0.6~0.9MPa；
S4, annealing: the sample through blasting treatment is annealed under 1000~1100 DEG C of argon atmosphere, and examination is taken out in furnace cooling
Sample；
It is S5, laser impact intensified: the sample of annealed processing to be subjected to laser-impact processing, the single pulse energy of laser-impact is
4~7J, spot diameter are 2.6~3mm, laser-impact number 1~3 time, are modified Ovshinsky after laser impact intensified processing
Body stainless steel.
The preparation method of the excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the step S2
In, the solid powder penetration enhancer includes the homogeneous mixture of following components: granularity is the aluminium powder of 200 mesh, Al2O3It is formed with Cr powder
Filler and its powdered NH4The penetration-assisting agent of Cl in the solid powder penetration enhancer, is counted in mass ratio, and the aluminium powder accounts for 42~
74%, the Al2O3Powder accounts for 20~40%, and the Cr powder accounts for 5~15%, the NH4Cl accounts for 1~3%.
The preparation method of the excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the step S4
In, the time of the annealing is 0.5~3h.
The preparation method of the excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the step S5
In, using pulse intensity laser device, using friction tape as protective layer, using water as restraint layer；The wavelength of laser is 1064nm, pulsewidth
For 10~30ns, overlapping rate 40~70%；The laser-impact processing is double-sided laser shock treatment；The laser-impact processing
Path direction it is vertical with the rolling direction of stainless steel materials.
The preparation method of the excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the step S3
In, the abrasive material of the sandblasting is the Al of 300~500 mesh2O3Particle；The time of the sandblasting is 5~20min, the distance 2 of sandblasting
~6cm.
The preparation method of the excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that the step S1
In, electrolyte includes the concentrated sulfuric acid that volume fraction is 60~80%, and the concentrated phosphoric acid and volume fraction that volume fraction is 15~37% are 3
~5% distilled water；The DC voltage of electrolysis is 5~6V, and the temperature of electrolyte is 60~80 DEG C, the time of electrobrightening is 2~
5min。
The preparation method of the excellent modification austenitic stainless steel of above-mentioned high temperature creep resistance, it is preferable that in the step
Before S1, further include the steps that carrying out the austenitic stainless steel surface mechanical polishing processing；The surface mechanical polishing is specific
Include: using 80 mesh~1200 mesh granularities sand paper be polishing to naked eyes it is visible without obvious scratch, then in ultrasonic wave use third
Ketone cleans 5~20min, oil removing, and dehydrated alcohol 5~20min of ultrasonic cleaning goes stain, is finally putting into 80 DEG C of dryings 20 of drying box
~40min.
Compared with the prior art, the advantages of the present invention are as follows:
1, modification austenitic stainless steel of the invention is due to excellent institutional framework, so that its tool is in melting aluminum alloy
Under conditions of high temperature stress, there is excellent creep-resistant property, and the strength of materials and toughness are high, by from by matrix surface
Successively include from the inside to the outside with a thickness of 40~80 μm the Fe phase diffusion layer containing Al, with a thickness of 50~100 μm of Fe-Al compounds
Layer and with a thickness of 10~20 μm of Al2O3The composition of the institutional framework of film, infiltration layer are free of brittlement phase, and even tissue, thickness can
Control, the component between infiltration layer and infiltration layer seamlessly transit in gradient, significantly reduce the interfacial stress and group between matrix and infiltration layer
Defect is knitted, the binding force between matrix and infiltration layer is effectively improved, inhibits infiltration layer to fall off, inhibit crack initiation and propagation, effectively mentions
Creep-resistant property of high 321 austenitic stainless steel under conditions of melting aluminum alloy and high temperature stress is able to satisfy based on melting
Alusil alloy is the work requirements of the solar energy thermal-power-generating heat exchanger tube of heat-storage medium, great learning value and commercial application potentiality.
2, Fe is free of in the infiltration layer of modification austenitic stainless steel of the invention2Al5、FeAl3Equal brittlement phases, bearing capacity is strong,
Adhesiveness between infiltration layer and between infiltration layer and matrix is good, it is not easy to peel off.
3, it is tightly combined between modification austenitic stainless steel infiltration layer of the invention, free from flaw, boundary are obvious and neat, infiltration layer
Surface hardness be 625~1390HV, invigoration effect depth be 300~1600 μm, the surface peening effect of material is good.
4, the present invention passes through specific electrobrightening, aluminising, sandblasting, annealing and these laser impact intensified processing steps
It organically combines in a specific sequence and 321 stainless steels is handled, and control aluminising temperature, blasting pressure, annealing temperature, laser
The parameters such as path, simple venation energy and spot intensity are impacted, are obtained from the Al for being followed successively by 10~20 μm inward outside2O3Film, 50~
Fe-Al compound layer (FeAl, FeAl of 100 μ m-thicks2And Fe3Al) and Al (Fe) the phase diffusion layer that contains of 40~80 μ m-thicks (contains Al
Fe phase diffusion layer) infiltration layer, be tightly combined between infiltration layer, free from flaw, boundary are obvious and neat, the stress between each interface
It is small, matrix and infiltration layer interfacial stress be small, layer surface macro morphology preferably, tissue crystal grain it is tiny, flawless, even tissue are thick
It spends controllably, without Fe2Al5、FeAl3The modification austenite that component between equal brittlement phases, infiltration layer and infiltration layer seamlessly transits in gradient is not
Become rusty steel, significantly reduces the interfacial stress and tissue defects between matrix and infiltration layer, effectively improves the knot between matrix and infiltration layer
With joint efforts, inhibit infiltration layer fall off, inhibit crack initiation and propagation, effectively improve 321 austenitic stainless steels melting aluminum alloy with
Creep-resistant property under conditions of high temperature stress resists under conditions of melting aluminum alloy and high temperature stress with excellent
Croop property, and austenitic stainless steel matrix strength and toughness can be improved.
5, method of the invention is by further controlling annealing time, penetration enhancer composition, the technological parameter of laser-impact, sandblasting
The technological parameters such as time, sandblasting distance, the condition of electrobrightening, can be further improved the control accuracy to tissue, thus into one
Step improves the compactness and integrality of tissue, obtains the modification austenite that surface peening is good and matrix toughness is high, effectively improves and change
The performances such as creep-resistant property, toughness and intensity of the property austenitic stainless steel under conditions of melting aluminum alloy and high temperature stress.
6, method of the invention is before electrobrightening by carrying out surface mechanical polishing processing to austenite stainless steel curved beam,
The impurity and covering for removing specimen surface, improve the cleanliness of specimen surface, handle the surface created for subsequent aluminising
Condition.
Detailed description of the invention
Fig. 1 is the laser impact intensified path profile that austenite stainless steel curved beam of the invention carries out laser-impact processing.
321 austenitic stainless steel of modification and 321 non-modified austenitic stainless steels prepared by Fig. 2 embodiment of the present invention 3
XRD comparison diagram.
Fig. 3 is the Cross Section Morphology of 321 austenitic stainless steel of modification prepared by the embodiment of the present invention 3 and the EDS energy of corresponding points
Spectrum analysis figure.
Fig. 4 is the microhardness of 321 austenitic stainless steel of modification prepared by the embodiment of the present invention 3 along depth of penetration direction
Variation diagram.
Fig. 5 is 321 austenitic stainless steel of modification prepared by the embodiment of the present invention 3 and 321 non-modified austenite stainless
High-temerature creep contrast curve chart of the steel at 620 DEG C/210MPa and at 620 DEG C/210MPa of melting aluminum alloy environment.
Specific embodiment
The present invention is described in further details below with reference to Figure of description and specific embodiment.
A kind of modification austenitic stainless steel that high temperature creep resistance of the invention is excellent, the modified austenitic stainless steel by
It is interior to outer include austenitic stainless steel matrix, with a thickness of 40~80 μm of the Fe phase diffusion layers containing Al, with a thickness of 50~100 μm
Fe-Al compound layer and 10~20 μ m-thicks Al2O3Film.
The Fe-Al compound layer is the non-brittle intermetallic compound of Fe and Al, including FeAl, FeAl2And Fe3Al。
The austenite stainless steel matrix is 321 austenitic stainless steels.
A kind of preparation method for the modification austenitic stainless steel that high temperature creep resistance of the invention is excellent, including following step
It is rapid:
(1) surface mechanically polishes: hot rolled plate austenite stainless steel plate is polishing to meat through different grain size (80~1200#) sand paper
Eye is visible without obvious scratch, then cleans 5~20min, oil removing, dehydrated alcohol ultrasonic cleaning 5 using acetone in ultrasonic wave
~20min, goes stain, is finally putting into 80 DEG C of drying box dry 20~40min；Wherein 321 austenitic stainless steels are rolled plates,
The mass fraction of chemical component is C 0.04%, Si 0.38%, Mn 1.08%, Cr 17.02%, Ni 9.06%, N 0.05%, P
0.03%, Ti 0.22%, remaining is Fe.Mechanical property under 321 stainless steel room temperature are as follows: 667 MPa of tensile strength (σ b), surrender
245 MPa of intensity (σ 0.2), elongation percentage 56.5%, hardness 175HV.
(2) electrobrightening: 321 austenite stainless steel plates are connect in anode, cathode with insoluble conductive material (graphite plate),
Anode and cathode spacing 50mm, electrolyte are heated to 60~80 DEG C (can pass through heating water bath), are passed through 5~6V DC voltage, are being electrolysed
After 2~5min of middle polishing, austenite stainless steel plate is taken out into bath cleaning drying, wherein the ingredient of electrolyte is as follows: volume point
The concentrated sulfuric acid (purity 98%) that number is 60~80%, the concentrated phosphoric acid (purity 85%) and volume fraction that volume fraction is 15~37%
For 3~5% distilled water.
(3) aluminising: solid powder penetration enhancer is made of silicon source, filler, penetration-assisting agent (activator), and wherein silicon source uses granularity
For the aluminium powder of 200 mesh, Al2O3Making filler with Cr powder is and powdered NH4The penetration-assisting agent of Cl forms, according to 5~15wt.%Cr,
42~74wt.%Al, 20~40wt.%Al2O3, 1~3wt.%NH4Cl is sufficiently mixed.By penetration enhancer and through the austenite of electrobrightening
Stainless steel plate is fitted into heat-resistance stainless steel batch can, is compressed, and fire clay sealing carries out aluminising: heating up with furnace, in 150 DEG C of dry 2h,
Then in 400~600 DEG C of 20~40min of heat preservation, heating rate is 10 DEG C/min, then in 900 DEG C~1050 DEG C 10~15h of heat preservation
After cool to room temperature with the furnace.
(4) blasting treatment: the austenite stainless steel plate after aluminising is placed under 0.6~0.9MPa high pressure nitrogen and is sprayed
Sand, abrasive material are the Al of 300~500 mesh2O3Particle, 5~20min of blast time, sandblasting 2~6cm of distance remove loose infiltration layer
And impurity.
(5) it anneals: the austenite stainless steel plate through aluminising is put into vacuum tube furnace, it is high-purity at 1000~1100 DEG C
0.5~3h of annealing time under argon gas, furnace cooling are taken out.
(6) laser impact intensified: the processing of double-sided laser shock peening, laser are carried out to the austenite stainless steel plate after annealing
Wavelength is 1064nm, and single pulse energy is 4~7J, and pulsewidth is 10~30ns, and spot diameter is 2.6~3mm, overlapping rate 40~
70%, friction tape is protective layer, and water is restraint layer, laser-impact number 1~3 time (can be 1 time, 2 times or 3 times).Fig. 1 is sharp
Light shock peening path, the path direction are vertical with the rolling direction of stainless steel materials.
The modification austenitic stainless steel and preparation method of enhancing resist melt alusil alloy high temperature creep property of the invention, it is right
After austenitic stainless steel aluminising after carrying out laser-impact, layer surface macro morphology is preferable, and tissue crystal grain is tiny, and nothing is split
Line.Infiltration layer is multilayered structure, from being successively uneven 10~20 μm of Al respectively inward outside2O3Film, 50~100 μ m-thicks
Fe-Al compound (FeAl, FeAl2And Fe3Al), 40~80 μ m-thicks contain Al (Fe) phase diffusion layer and matrix.And between infiltration layer
It is tightly combined, free from flaw, boundary are obvious and neat.The surface hardness of infiltration layer is 625~1390HV, and invigoration effect depth is 300
~1600 μm.Under 620 DEG C of melting aluminum alloy environment, the high temperature tensile creep rupture time under 210MPa creep loading is 94h
More than, secondary creep rates 1.1254x10-7Hereinafter, (creep fracture time 73h, secondary creep rates compared with 321 rust steel
For 2.7143x10-7), secondary creep rates substantially reduce, and show excellent resist melt alusil alloy high temperature creep property, full
Work requirements of the foot based on the solar energy thermal-power-generating heat exchanger tube that melting aluminum alloy is heat-storage medium, great learning value and industry
Application potential.
Embodiment 1:
A kind of preparation method for the modification austenitic stainless steel that high temperature creep resistance of the invention is excellent, comprising the following steps:
(1) surface mechanically polishes: by hot rolled plate austenite stainless steel plate sample through different grain size (80 mesh~1200 mesh) sand paper
It is visible without obvious scratch to be polishing to naked eyes, 5min is then cleaned using acetone in ultrasonic wave, oil removing, dehydrated alcohol ultrasonic wave is clear
5min is washed, stain is gone, is finally putting into 80 DEG C of drying box dry 20min；Wherein 321 austenitic stainless steels are rolled plates, chemistry
The mass fraction of ingredient be C 0.04%, Si 0.38%, Mn 1.08%, Cr 17.02%, Ni 9.06%, N 0.05%, P 0.03%,
Ti 0.22%, remaining is Fe.Condition of heat treatment: the mechanical property under 321 stainless steel room temperature are as follows: tensile strength (σb) it is 667
MPa, yield strength (σ0.2) it is 245 MPa, elongation percentage 56.5%, hardness 175HV.
(2) electrobrightening: 321 austenite stainless steel plates are connect in anode, cathode with insoluble conductive material (graphite plate),
Anode and cathode spacing 50mm, electrolyte are heated to 60 DEG C, and the two poles of the earth enter in electrolyte simultaneously, 5V DC voltage are passed through, in electrolysis
2min is impregnated, sample takes out bath cleaning drying；The concentrated sulfuric acid (purity 98%) that the ingredient of electrolyte is 60% by volume fraction,
The distilled water composition that the concentrated phosphoric acid (purity 85%) and volume fraction that volume fraction is 37% are 3%.
(3) aluminising: solid powder penetration enhancer is made of silicon source, filler, penetration-assisting agent (activator), and wherein silicon source uses granularity
For the aluminium powder of 200 mesh, Al2O3Making filler with Cr powder is and powdered NH4The penetration-assisting agent of Cl forms, according to 5wt.%Cr,
64wt.%Al, 28wt.%Al2O3, 3wt.%NH4Cl is sufficiently mixed.Penetration enhancer and sample are fitted into heat-resistance stainless steel batch can, compressed,
Fire clay sealing, carries out aluminising: heating up with furnace, 150 DEG C of dry 2h, 400 DEG C of heat preservation 20min, and heating rate is 10 DEG C/min,
Room temperature is cooled to the furnace after 900 DEG C of heat preservation 15h.
(4) blasting treatment: sample after aluminising being placed under 0.6MPa high pressure nitrogen and carries out sandblasting, and abrasive material is 300 purposes
Al2O3Particle, blast time 5min, sandblasting distance 6cm remove loose infiltration layer and impurity.
(5) it anneals: aluminising sample being put into vacuum tube furnace, the annealing time 1.5h under high-purity argon gas at 1000 DEG C,
Sample is taken out in furnace cooling.
(6) laser impact intensified: the processing of double-sided laser shock peening to be carried out to aluminising stainless steel, optical maser wavelength is
1064nm, single pulse energy 4J, pulsewidth 10ns, spot diameter 2.8mm, overlapping rate 40%, friction tape are protective layer, water
For restraint layer, laser-impact number 1 time.The path direction of laser-impact processing is vertical with the rolling direction of stainless steel materials.
Infiltration layer obtained and matrix and Coating combination is close, infiltration layer is from being successively rough 20 μm respectively inward outside
Thick Al2O3Fe-Al compound layer (FeAl, FeAl of film, 80~100 μ m-thicks2And Fe3Al), 60~70 μ m-thicks containing Al's
Fe phase diffusion layer and matrix, infiltration layer is interior to be free of Fe2Al5、FeAl3Equal brittlement phases.The surface hardness of infiltration layer is 600~700HV,
Invigoration effect depth is 300~400 μm.
Embodiment 2:
A kind of preparation method for the modification austenitic stainless steel that high temperature creep resistance of the invention is excellent, comprising the following steps:
(1) surface mechanically polishes: hot rolled plate austenite stainless steel curved beam is beaten through different grain size (80 mesh~1200 mesh) sand paper
It is visible without obvious scratch to be milled to naked eyes, 10min is then cleaned using acetone in ultrasonic wave, oil removing, dehydrated alcohol ultrasonic wave is clear
10min is washed, stain is gone, is finally putting into 80 DEG C of drying box dry 30min；Wherein 321 austenitic stainless steels are rolled plates, chemistry
The mass fraction of ingredient be C 0.04%, Si 0.38%, Mn 1.08%, Cr 17.02%, Ni 9.06%, N 0.05%, P 0.03%,
Ti 0.22%, remaining is Fe.Mechanical property under 321 stainless steel room temperature are as follows: tensile strength (σb) it is 667 MPa, yield strength
(σ0.2) it is 245 MPa, elongation percentage 56.5%, hardness 175HV.
2) electrobrightening: 321 austenitic stainless steels are connect in anode, cathode insoluble conductive material (graphite plate), yin
Anode spacing 50mm, electrolyte are heated to 70 DEG C, and the two poles of the earth enter in electrolyte simultaneously, are passed through 5V DC voltage, soak in electrolysis
5min is steeped, sample takes out bath cleaning drying, wherein (purity is the concentrated sulfuric acid that the ingredient of electrolyte is 70% by volume fraction
98%) the distilled water composition that the concentrated phosphoric acid (purity 85%) and volume fraction that, volume fraction is 26% are 4%.
(3) aluminising: solid powder penetration enhancer is made of silicon source, filler, penetration-assisting agent (activator), and wherein silicon source uses granularity
For the aluminium powder of 200 mesh, Al2O3Making filler with Cr powder is and powdered NH4The penetration-assisting agent of Cl forms, according to 15wt.%Cr,
44wt.%Al, 40wt.%Al2O3, 1wt.%NH4Cl is sufficiently mixed.Penetration enhancer and sample are fitted into heat-resistance stainless steel batch can, pressed
Tightly, fire clay seal, carry out aluminising: heat up with furnace, 150 DEG C of dry 2h, 600 DEG C of heat preservation 40min, heating rate for 10 DEG C/
Min cools to room temperature with the furnace after 1050 DEG C of heat preservation 10h.
(4) blasting treatment: sample after aluminising being placed under 0.8MPa high pressure nitrogen and carries out sandblasting, and abrasive material is 400 purposes
Al2O3Particle, blast time 10min, sandblasting distance 4cm remove loose infiltration layer and impurity.
(5) it anneals: aluminising sample being put into vacuum tube furnace, the annealing time 0.5h under high-purity argon gas at 1100 DEG C,
Sample is taken out in furnace cooling.
(6) laser impact intensified: the processing of double-sided laser shock peening to be carried out to aluminising stainless steel, optical maser wavelength is
1064nm, single pulse energy 6J, pulsewidth 30ns, spot diameter 3mm, overlapping rate 70%, friction tape are protective layer, and water is
Restraint layer, laser-impact number 3 times.Fig. 1 is the laser impact intensified path of the present embodiment, the path direction and stainless steel materials
Rolling direction it is vertical.
Infiltration layer obtained and matrix and Coating combination is close, infiltration layer is from being successively rough 10 μm respectively inward outside
Thick Al2O3Fe-Al compound layer (FeAl, FeAl of film, 70~80 μ m-thicks2And Fe3Al), the Fe containing Al of 50~60 μ m-thicks
Phase diffusion layer and matrix, infiltration layer is interior to be free of Fe2Al5、FeAl3Equal brittlement phases.The surface hardness of infiltration layer is 700~800HV, by force
Changing depth of interaction is 800~1400 μm.
Embodiment 3:
A kind of preparation method for the modification austenitic stainless steel that high temperature creep resistance of the invention is excellent, comprising the following steps:
(1) surface mechanically polishes: hot rolled plate austenite stainless steel curved beam is beaten through different grain size (80 mesh~1200 mesh) sand paper
It is visible without obvious scratch to be milled to naked eyes, 20min is then cleaned using acetone in ultrasonic wave, oil removing, dehydrated alcohol ultrasonic wave is clear
20min is washed, stain is gone, is finally putting into 80 DEG C of drying box dry 40min；Wherein 321 austenitic stainless steels are rolled plates, chemistry
The mass fraction of ingredient be C 0.04%, Si 0.38%, Mn 1.08%, Cr 17.02%, Ni 9.06%, N 0.05%, P 0.03%,
Ti 0.22%, remaining is Fe.Mechanical property under 321 stainless steel room temperature are as follows: tensile strength (σ b) is 667 MPa, yield strength
(σ 0.2) is 245 MPa, elongation percentage 56.5%, hardness 175HV.
(2) electrobrightening: 321 austenitic stainless steels are connect in anode, cathode insoluble conductive material (graphite plate), yin
Anode spacing 50mm, electrolyte are heated to 80 DEG C, and the two poles of the earth enter in electrolyte simultaneously, are passed through 5V DC voltage, soak in electrolysis
3min is steeped, sample takes out bath cleaning drying；The concentrated sulfuric acid (purity 98%) of the ingredient of electrolyte by volume fraction 80%, volume
The distilled water composition for the concentrated phosphoric acid (purity 85%) and volume fraction 5% that score is 15%.
(3) aluminising: solid powder penetration enhancer is made of silicon source, filler, penetration-assisting agent (activator), and wherein silicon source uses granularity
For the aluminium powder of 200 mesh, Al2O3Making filler with Cr powder is and powdered NH4The penetration-assisting agent of Cl forms, according to 10wt.%Cr,
58wt.%Al, 30wt.%Al2O3, 2wt.%NH4Cl is sufficiently mixed.Penetration enhancer and sample are fitted into heat-resistance stainless steel batch can, compressed,
Fire clay sealing, carries out aluminising: heating up with furnace, 150 DEG C of dry 2h, 500 DEG C of heat preservation 30min, and heating rate is 10 DEG C/min,
Room temperature is cooled to the furnace after 950 DEG C of heat preservation 12h.
(4) blasting treatment: sample after aluminising being placed under 0.9MPa high pressure nitrogen and carries out sandblasting, and abrasive material is 500 purposes
Al2O3Particle, blast time 5min, sandblasting distance is 2cm, removes loose infiltration layer and impurity.
(5) it anneals: aluminising sample being put into vacuum tube furnace, the annealing time 1h under high-purity argon gas at 1050 DEG C, with
Furnace is cooling to take out sample.
(6) laser impact intensified: double-sided laser intensive treatment is carried out to aluminising stainless steel using pulse intensity laser device,
Optical maser wavelength is 1064nm, single pulse energy 7J, pulsewidth 20ns, spot diameter 2.6mm, overlapping rate 50%, and friction tape is
Protective layer, water are restraint layer, laser-impact number 3 times.Fig. 1 is the laser impact intensified path of the present embodiment, the path direction
It is vertical with the rolling direction of stainless steel materials.
XRD analysis is carried out to infiltration layer made from the present embodiment, result is as shown in Fig. 2, infiltration layer object phase composition ingredient is main
By FeAl, FeAl2And Fe3Al composition, infiltration layer is interior to be free of Fe2Al5、FeAl3Equal brittlement phases.
Sem analysis is carried out to infiltration layer made from the present embodiment, result is as shown in figure 3, infiltration layer and matrix and interlayer knot
Conjunction is close, free from flaw, boundary are obvious and neat, illustrates that aluminized coating and matrix have formed metallurgical bonding, as shown in Fig. 3 (a), edge is seeped
Layer depth direction by taking tetra- points of A, B, C, D inward outside, and EDS figure is successively such as Fig. 3 (b), 3(c), 3(d), 3(e) shown in (i.e. Fig. 3
In, (a) is Cross Section Morphology；It (b) is the corresponding EDS power spectrum of A point；It (c) is the corresponding EDS power spectrum of B point；(d) corresponding for C point
EDS power spectrum；(e) it is the corresponding EDS power spectrum of D point), wherein Al constituent content gradually decreases, and Fe constituent content gradually increases.Infiltration layer
From being successively rough 10 μ m-thick Al respectively inward outside2O3Film, 50~60 μ m-thicks Fe-Al compound (including FeAl,
FeAl2And Fe3Al), the Fe phase diffusion layer and matrix containing Al of 40~50 μ m-thicks.
Fig. 4 is variation of the microhardness made from the present embodiment with depth of penetration direction, and surface microhardness is
1390HV is 7.95 times of 321 stainless steel hardness (175HV) before modified, and invigoration effect depth is up to 1600 μm.
Fig. 5 is that modified 321 austenitic stainless steels and 321 non-modified austenitic stainless steels made from the present embodiment exist
High temperature compressed creep curve under 620 DEG C/210MPa creep loading, and it is compacted in melting aluminum alloy environment, 620 DEG C/210MPa
High temperature compressed creep curve comparison diagram under varying load.As shown in Figure 5, high temperature of 321 stainless steels at 620 DEG C, 210MPa is compacted
Become rupture time 105h, secondary creep rates are 1.3285 × 10-7, under identical creep loading (210MPa), melting aluminum alloy
321 stainless steel creep-resistant properties can be reduced, corresponding creep fracture time is 73h, secondary creep rates under melting aluminum environment
It is 2.7143 × 10-7；And creep of modified 321 austenitic stainless steels in melting aluminum alloy environment made from the present embodiment is disconnected
Splitting the time is 124h, and secondary creep rates are 6.0575 × 10-8, compared with 321 rust steel, creep-resistant property improves 1 order of magnitude；
(creep fracture time is simultaneously compared with the common high temperature creep property of modified 321 austenitic stainless steels made from the present embodiment
128h), the influence of molten aluminium alloy environment is negligible.
Although the present invention is disclosed as above with preferred embodiment, however, it is not intended to limit the invention.It is any to be familiar with ability
The technical staff in domain, without deviating from the scope of the technical scheme of the present invention, all using the technology contents pair of the disclosure above
Technical solution of the present invention makes many possible changes and modifications or equivalent example modified to equivalent change.Therefore, all
Without departing from the content of technical solution of the present invention, according to the present invention technical spirit any simple modification made to the above embodiment,
Equivalent variations and modification, all shall fall within the protection scope of the technical scheme of the invention.
Claims (10)
1. the excellent modification austenitic stainless steel of high temperature creep resistance, which is characterized in that the modified austenitic stainless steel includes
Austenite stainless steel matrix and infiltration layer, the infiltration layer include from the inside to the outside with a thickness of 40~80 μm the Fe phase diffusion layer containing Al,
Fe-Al compound layer with a thickness of 50~100 μm and the Al with a thickness of 10~20 μm2O3Film.
2. the excellent modification austenitic stainless steel of high temperature creep resistance as described in claim 1, which is characterized in that the Fe-
Al compound layer is the non-brittle intermetallic compound of Fe and Al；The non-brittle intermetallic compound includes FeAl, FeAl2With
Fe3Al。
3. the excellent modification austenitic stainless steel of high temperature creep resistance as claimed in claim 1 or 2, which is characterized in that described
Austenite stainless steel matrix is 321 austenitic stainless steels；The surface hardness of the infiltration layer is 625~1390HV, and invigoration effect is deep
Degree is 300~1600 μm.
4. the preparation method of the excellent modification austenitic stainless steel of high temperature creep resistance, which comprises the steps of:
S1, electrobrightening: using austenitic stainless steel as anode, using insoluble conductive material as cathode, to austenitic stainless steel into
The processing of row electrobrightening；
S2, aluminising: being dried the austenitic stainless steel handled through electrobrightening, then is seeped using solid powder penetration enhancer
Aluminium, the condition of the aluminising are as follows: prior to 400~600 DEG C 20~40min of heat preservation, then at 900 DEG C~1050 DEG C 10~15h of heat preservation
After cool to room temperature with the furnace；
S3, blasting treatment: the austenitic stainless steel after aluminising is subjected to sandblasting under the high pressure nitrogen of 0.6~0.9MPa；
S4, annealing: the austenitic stainless steel through blasting treatment is annealed under 1000~1100 DEG C of argon atmosphere, furnace cooling
After take out；
It is S5, laser impact intensified: the austenitic stainless steel of annealed processing is subjected to laser-impact processing, the simple venation of laser-impact
Rush energy be 4~7J, spot diameter be 2.6~3mm, laser-impact number 1~3 time, after laser impact intensified processing to get
Modified austenitic stainless steel.
5. the preparation method of the excellent modification austenitic stainless steel of high temperature creep resistance as claimed in claim 4, feature exist
In in the step S2, the solid powder penetration enhancer includes the homogeneous mixture of following components: granularity is the aluminium powder of 200 mesh,
Al2O3With the filler and its powdered NH of Cr powder composition4The penetration-assisting agent of Cl in the solid powder penetration enhancer, is counted in mass ratio,
The aluminium powder accounts for 42~74%, the Al2O3Powder accounts for 20~40%, and the Cr powder accounts for 5~15%, the NH4Cl accounts for 1~3%.
6. the preparation method of the excellent modification austenitic stainless steel of high temperature creep resistance as claimed in claim 4, feature exist
In in the step S4, the time of the annealing is 0.5~3h.
7. the preparation method of the excellent modification austenitic stainless steel of high temperature creep resistance as claimed in claim 4, feature exist
In in the step S5, using pulse intensity laser device, using friction tape as protective layer, using water as restraint layer；The wavelength of laser
For 1064nm, pulsewidth is 10~30ns, overlapping rate 40~70%；The laser-impact processing is double-sided laser shock treatment；It is described
The path direction of laser-impact processing is vertical with the rolling direction of stainless steel materials.
8. the preparation side of the excellent modification austenitic stainless steel of high temperature creep resistance as described in claim 4~7 any one
Method, which is characterized in that in the step S3, the abrasive material of the sandblasting is the Al of 300~500 mesh2O3Particle；The sandblasting when
Between be 5~20min, 2~6cm of distance of sandblasting.
9. the preparation side of the excellent modification austenitic stainless steel of high temperature creep resistance as described in claim 4~7 any one
Method, which is characterized in that in the step S1, electrolyte include volume fraction be 60~80% the concentrated sulfuric acid, volume fraction be 15~
The distilled water that 37% concentrated phosphoric acid and volume fraction is 3~5%；The DC voltage of electrolysis is 5~6V, the temperature of electrolyte is 60~
80 DEG C, the time of electrobrightening is 2~5min.
10. the preparation side of the excellent modification austenitic stainless steel of high temperature creep resistance as described in claim 4~7 any one
Method, which is characterized in that further include the step that surface mechanical polishing processing is carried out to the austenitic stainless steel before the step S1
Suddenly；The surface mechanical polishing specifically includes: being polishing to the visible nothing of naked eyes using 80 mesh~1200 mesh granularities sand paper and obviously draws
Trace, then cleans 5~20min, oil removing using acetone in ultrasonic wave, and dehydrated alcohol 5~20min of ultrasonic cleaning goes stain, most
Afterwards in 80 DEG C of dry 20~40min.
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| CN112458398A (en) * | 2020-11-25 | 2021-03-09 | 浙江申久金属制品有限公司 | Preparation method of aluminized stainless steel plate assisted by sand blasting and stainless steel plate |
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| CN112080718B (en) * | 2020-08-24 | 2022-09-06 | 向双清 | Method for preparing FeAl-based intermetallic compound flexible membrane by Al infiltration |
| 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 |
| CN114231894B (en) * | 2021-12-01 | 2023-06-20 | 常州大学 | Low-temperature high-efficiency ion nitrogen aluminum co-permeation surface modification method |
| CN114231895A (en) * | 2021-12-15 | 2022-03-25 | 常州大学 | High-performance low-temperature high-efficiency ionic composite permeation surface modification method for austenitic stainless steel |
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