CN109023228A - Alloying Fe3The fused salt non-electrolytic preparation method of Si infiltration layer raising wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel - Google Patents
Alloying Fe3The fused salt non-electrolytic preparation method of Si infiltration layer raising wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/18—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions
- C23C10/20—Solid state diffusion of only metal elements or silicon into metallic material surfaces using liquids, e.g. salt baths, liquid suspensions only one element being diffused
- C23C10/24—Salt bath containing the element to be diffused
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Abstract
The invention discloses alloying Fe3Si infiltration layer improves the method that 2Cr13 martensitic stain less steel is wear-resisting, erosion resistant surface comprehensive performance fused salt non-electrolytic seeps preparation.The invention proposes two kinds of alloying Fe3The technology of preparation method of Si infiltration layer, one is prepared using the alloying elements cr in 2Cr13 matrix composition with well passivated performance, the Cr alloying siliconising layer that corrosion resistance is good and wearability is high；Another kind is first to prepare certain thickness Ni, Cu etc. in matrix surface by electro-plating method to design Plating System, has then obtained the alloyings Fe such as (Ni, Cr)-, (Cu, Cr)-through neutral fused salt non-electrolytic siliconising3Si infiltration layer.Using alloying Fe produced by the present invention3Si infiltration layer is firmly combined with 2Cr13 matrix, effectively raises the against corrosion and wear-resisting property of 2Cr13 steel, to meet the requirement of different work condition environments, and method is easy, low in cost, therefore has a good application prospect.
Description
Technical field
The invention belongs to surface metallurgic field of engineering technology, it is related to enhancing 2Cr13 martensitic stain less steel wear-resisting erosion resistance synthesis
The method of performance, in particular to a kind of alloying Fe3The fused salt of Si infiltration layer raising wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel
Non-electrolytic preparation method.
Background technique
2Cr13 martensitic stain less steel intensity with higher and mechanical performance, thus it is widely used in turbine blade, compression
The plasticity such as machine blade, fastener, anti-corrosion cutlery, bearing and the higher part of loading demands is absorbed impact, however itself is resistance to
Corrosion and wearability are still difficult to meet the requirement that industrial environment increasingly changes, and surface peening is that raising material comprehensive performance is most straight
Connect effective method.Currently, available method mainly has carburizing, low temperature plasma nitriding, laser surface modification etc..But ion seeps
Expensive equipment is needed with Laser Surface Treatment, not only temperature is high for High temperature ion carburizing, but also the preparation time period is especially long.For
This, seeks low cost, prepares the major issue that convenient technical method is always field of engineering technology.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the object of the present invention is to provide alloying Fe3Si infiltration layer improves
The fused salt non-electrolytic preparation method of wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel, this method can use the alloy inside steel
Change element or and obtains a kind of alloying Fe by adding exterior alloy element (electrodeposition of metals)3Si layers, it is made to can be used as one
Kind obdurability coating is utilized, and has many advantages, such as that simple process, synthesis temperature are low, soaking time is short, and gained infiltration layer and base
It is to be combined by forming alloy and (belong to metallurgical bonding), thus combination is very secured between body metal, infiltration layer is not easily to fall off, and sample
It is wrapped in wherein by fused salt, avoids contacted with oxygen during heating, surface is not easy to be oxidized.
To achieve the goals above, the technical solution adopted by the present invention is that:
Alloying Fe3Si infiltration layer improves the fused salt non-electrolytic preparation method of wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel,
Neutral fused salt siliconising preparation alloying is carried out to the 2Cr13 matrix containing Cr alloying element or with coated 2Cr13 matrix
Fe3Si layers.The alloying Fe that gained and matrix are firmly combined3Si infiltration layer, by the alloying Fe of surface compact3Si layers and phase under it
To two layers of diffusion layer loose porous composition.
Preferably, alloying Fe is prepared in neutral fused salt siliconising3Before Si layers, first 2Cr13 matrix is carried out to include surface
Sample, the disk of Ф 30mm × 8mm is cut by spark cutting method by the pretreatment of two Mechanical Planarization, oil removing links,
Then it being successively polishing to 1000# with waterproof abrasive paper is two-sided, then is cleaned by ultrasonic oil removing with acetone, the surface 2Cr13 is smooth after processing,
There is metallic luster, obtains no greasy dirt, the attachment of non-corroding object and the metal surface without obvious oxide layer.
Preferably, alloying Fe is prepared in neutral fused salt siliconising3Before Si layers, the design of alloying source is carried out, that is, according to not
Same work condition environment selects the different demands of surface property to carry out electro-deposition directly on 2Cr13 matrix or on the surface 2Cr13
The coating such as Ni or/and Cu are prepared, Ni or/and Cu and the more kinds of alloying sources matrix Cr are formed, to obtain higher surface generalization
Energy.Exterior alloy element Ni, Cu, which are introduced, using electro-deposition is able to achieve expansion regulation alloying Fe3Si penetrated layer property, wherein Ni has
There are good toughening effect and Cr to be used cooperatively the anti-corrosion and wear-resisting property that can effectively improve stainless steel, Cu has anti-carburizi ng, easily expands
Scattered effect can effectively slow down Si and Fe counterdiffusion rate, be expected to reduce the appearance of Ke Kendaer hole band.
Preferably, the thickness of coating is 5~20 μm, and coating is firmly combined with substrate, meets the requirement of coating gross.
Preferably, the fused salt is by neutral salt NaCl, KCl, NaF and siliconizing medium Na2Si6F, Si powder forms, in molar ratio
33%NaCl, 33%KCl, 14%NaF, 5%Na2SiF6, 15%Si configuration, before carrying out fused salt siliconising processing, by neutral salt
1h is dried at 100 DEG C, then is uniformly mixed with siliconizing medium and is ground into fine powder.
Preferably, in alloying Fe3In Si layers of preparation process, alloy source (matrix or/and alloy source coating) will be designed
2Cr13 sample be embedded in the fused salt mixt in alumina crucible, it is ensured that specimen surface and fused salt fine powder come into full contact with, quartz
Stick is also placed in fused salt vertically, to stablize the source Si penetration enhancer.
Preferably, in alloying Fe3In Si layers of preparation process, 700~830 DEG C of holding temperature of setting, soaking time 2~
4h.And the hardening heat of 2Cr13 martensitic stain less steel is between 980~1050 DEG C, so being warming up to 800 DEG C of heat preservation 4h simultaneously with furnace
It will not influence the variation that matrix itself is organized, it is a kind of good with high-bond and obdurability finally to have obtained on matrix surface
Alloying Fe3Si infiltration layer improves the comprehensive performance of matrix.
Preferably, alloying Fe3After the completion of Si layers of infiltration system, quickly quartz pushrod and 2Cr13 sample are taken out, 2Cr13 sample
Place in air after natural cooling, clean the residual salt on removal surface repeatedly with hot water, and with acetone and washes of absolute alcohol, take off
Water and drying.
The present invention is heated by the way that sample and quartz pushrod are fully embedded fused salt again after mixing by neutral salt and siliconizing medium
Prepare the Fe of alloying3Si protective layer, the process fused salt have completely cut off contact of the sample with air to a certain extent, have avoided table
The oxidation in face, and it is the process control, easy to operate, at low cost, and obtained infiltration layer compactness is preferable, is increasing surface hardness
Anti-corrosion and wear-resisting property is significantly improved simultaneously, alloying makes it while then avoiding intermetallic compound brittleness well
It is utilized as a kind of coating material.
Detailed description of the invention
Fig. 1 is the XRD spectra that combined processing rear surface is seeped in 2Cr13 matrix siliconising processing and plating.
Fig. 2 is the micro-structure diagram that infiltration layer section after combined processing is seeped in 2Cr13 matrix siliconising processing and plating, in which: (a)
Cr-Fe3Si section；(b)(Cu,Cr)-Fe3Si section；(c)(Ni,Cr)-Fe3Si section.
Fig. 3 is the polarization curve that infiltration layer after combined processing is seeped in 2Cr13 matrix siliconising processing and plating.
Fig. 4 is the AC impedance figure that infiltration layer after combined processing is seeped in 2Cr13 matrix siliconising processing and plating.
Fig. 5 is the friction factor figure that infiltration layer after combined processing is seeped in 2Cr13 matrix siliconising processing and plating.
Fig. 6 is the Volume Loss figure that infiltration layer after combined processing is seeped in 2Cr13 matrix siliconising processing and plating.
Specific embodiment
The embodiment that the present invention will be described in detail with reference to the accompanying drawings and examples.
Embodiment 1
2Cr13 matrix prepares Cr alloying Fe by fused salt siliconising3Si protective layer utilizes the conjunction in 2Cr13 matrix composition
Gold element Cr prepares with well passivated performance, the Cr alloying siliconising layer that corrosion resistance is good and wearability is high, and specific steps are such as
Under:
1) material the pre-treatment of 2Cr13 matrix: is cut into 8mm thickness by spark cutting method from the bar of φ 30mm
Circular disc test specimen, surface is then super with acetone successively through the two-sided polishing of 240#, 400#, 600#, 800#, 1000# metallographic waterproof abrasive paper
Sound cleans 10min, then dries after being dehydrated with dehydrated alcohol, keeps surface smooth, there is metallic luster.
2) fused salt seeps preparation Cr alloying Fe3Si.Fused salt is by neutral salt NaCl, KCl, NaF and siliconizing medium Na2Si6F, Si powder
Composition, each reagent are that analysis is pure.Firstly, neutral salt is put into vacuum oven dry 1h at 100 DEG C.Then, it then and seeps
Silicea is uniformly mixed, and ground at fused salt fine powder, loading alumina crucible, and ready sample is embedded in fused salt.
It is finally inserted vertically into quartz pushrod (for supplementing element silicon in fused salt) in crucible, is put into chamber type electric resistance furnace and is heated to 750 DEG C
After keep the temperature 4h.Sample is taken out from fuse salt after completing siliconising, uses the residual salt in deionized water washed samples surface after being air-cooled to room temperature,
It is cleaned by ultrasonic again through acetone, is dried after dehydrated alcohol dehydration.
The XRD spectra schematic diagram of 1 layer surface of embodiment is as shown in Figure 1, infiltration layer main phase ingredient is the Fe of alloying3Si,
Secondly there are also a small amount of SiO2, cross-section structure is as shown in Fig. 2, wherein (a) is Cr-Fe3Si section；It (b) is (Cu, Cr)-Fe3Si
Section；It (c) is (Ni, Cr)-Fe3Si section, it is seen that infiltration layer by surface layer densification alloying Fe3Si layers and its under it is loose porous
Diffusion layer composition.
There is Cr alloying Fe with prepared by embodiment 13The sample of Si protective layer is working electrode, and platinum electrode is auxiliary electricity
Pole, saturated calomel electrode are reference electrode, under room temperature, in 10Vol.%H2SO4Middle p-wire polarization curve, take-off potential
For -0.8~0.6V, sweep speed 1mV/s, as shown in figure 3, compared with matrix, infiltration layer has apparent blunt obtained result
Change characteristic, corrosion potential increases, and corrosion current density reduces, and effectively raises the corrosion resistance to sulfuric acid of matrix.
There is Cr alloying Fe with prepared by embodiment 13The sample of Si protective layer is working electrode, using AC impedance skill
The chemical property of art test electrode.Alloying Fe3For Si infiltration layer sample as working electrode, platinum electrode is auxiliary electrode, saturation
Potassium chloride calomel electrode is reference electrode, under room temperature, in 10Vol.%H2SO4In tested, frequency range 100kHz
~10mHz, 10mV sine wave are as pumping signal.It is as shown in Figure 4 with the ac impedance spectroscopy comparison of matrix, it can be seen that infiltration layer
Capacitive reactance arc radius is about 4 times of matrix, illustrates that the corrosion resistance of infiltration layer is more preferable, this is consistent with polarization curve test result.
The Cr alloying Fe prepared with embodiment 13Si protective layer and 2Cr13 matrix carry out ball-disk friction mill as a comparison
Damage test, load 5N, abrasive material Al2O3, it is 60min to time consuming, friction factor changes over time curve such as Fig. 5 institute
Show, it can be seen that infiltration layer has the coefficient of friction lower than substrate, belongs to antifriction surface, wear volume it is weightless as shown in fig. 6,
Fe3Si protective layer makes the wear volume loss of substrate be reduced to 1/12, so effectively increasing the wear-resisting property of substrate.
Embodiment 2
Plating seeps combined processing and prepares multi-element alloyed Fe3Si protective layer first prepares one in matrix surface by electro-plating method
Determine the design Plating System such as Ni, Cu of thickness, then obtains (Ni, Cr)-, (Cu, Cr)-etc. through neutral fused salt non-electrolytic siliconising
Alloying Fe3Si infiltration layer, the specific steps are as follows:
1) pre-treatment of 2Cr13 matrix: with the in embodiment 1 1) step.
2) deposit N i and Cu coating: zinc coat thickness control is usually realized in 8~10 μm by introducing exterior alloy member
It is multi-element alloyed, achieve the purpose that improve substrate performance.
3) fused salt siliconising is handled: with the in embodiment 1 the 2) step, having obtained (Ni, Cr)-, (Cu, Cr)-alloying Fe3Si is anti-
Sheath.
To embodiment 2 plate seep combined processing obtained by alloying layer carry out material phase analysis, XRD analysis result as shown in Figure 1,
From diffracting spectrum as can be seen that infiltration layer main phase is alloying Fe3Si, diffraction maximum and standard PDF card (35-0519) are good
Unanimously, in addition, in addition to main phase ingredient Fe3There are small amounts object NiO and Cu64O generation respectively on the outer infiltration layer of Si, wherein the oxygen of Ni
Compound is one of the main component of stainless steel passivating film in acid condition, this can have excellent enhancing to make to corrosion resistance of surface
With.Cross-section structure is as shown in Fig. 2, in contrast, plating infiltration combined processing is got well than direct siliconising gained infiltration layer compactness, and Ke Ken
Da Er hole band significantly reduces.
Ni-Cr the and Cu-Cr alloying Fe prepared with embodiment 23Si protective layer sample is working electrode, supplemented by platinum electrode
Electrode is helped, saturation potassium chloride calomel electrode is reference electrode, under room temperature, in 10Vol.%H2SO4Middle test linear polarization is bent
Line, take-off potential are -1~1V, and sweep speed 1mV/s, obtained result is fig. 3, it is shown that combined processing infiltration layer
With apparent passive behavior, Fe3Secondary passivity, Fe has occurred in Si (Cu)3Multiple passivation has occurred in Si (Ni), while having height
Corrosion potential in matrix and the corrosion current density lower than matrix, effectively increase the corrosion resistance to sulfuric acid of matrix.
Ni-Cr the and Cu-Cr alloying Fe prepared with embodiment 23Si protective layer sample is working electrode, is hindered using exchange
The chemical property of anti-technical testing electrode.Platinum electrode is auxiliary electrode, and saturated calomel electrode is reference electrode, room temperature condition
Under, in 10Vol.%H2SO4In tested, frequency range be 100kHz~10mHz, 10mV sine wave is as pumping signal.With
The ac impedance spectroscopy comparison of matrix is as shown in Figure 4, it can be seen that seeps Fe3The capacitive reactance arc radius of Si (Cu) layer is about the 2 of matrix
Times, Fe3Si (Ni) layer capacitive reactance arc radius is about 9 times of matrix, and the corrosion resistance of the infiltration layer after illustrating combined processing is more preferable, this with
Polarization curve test result is consistent.
Ni-Cr the and Cu-Cr alloying Fe prepared with embodiment 23Si protective layer sample and 2Cr13 matrix are that comparison carries out
Ball-on-disc testing machine, load 5N, abrasive material Al2O3, it is 60min to time consuming, friction factor changes over time
Curve is as shown in Figure 5, it can be seen that the infiltration layer of combined processing has the coefficient of friction lower than substrate, belongs to antifriction surface, wears
Volume Loss is as shown in fig. 6, Fe3Si (Cu) protective layer makes the wear volume loss of substrate be reduced to 1/15, Fe3Si (Cu) is anti-
Sheath makes the wear volume loss of substrate be reduced to 1/21, so the infiltration layer of combined processing effectively increases the wearability of substrate
Energy.
To sum up, the invention proposes two kinds of alloying Fe3The technology of preparation method of Si infiltration layer, one is utilize 2Cr13 base
Alloying elements cr in body ingredient prepares with well passivated performance, the Cr alloying siliconising that corrosion resistance is good and wearability is high
Layer；Another kind is first to prepare certain thickness Ni, Cu etc. in matrix surface by electro-plating method to design Plating System, is then passed through
Property fused salt non-electrolytic siliconising has obtained the alloyings Fe such as (Ni, Cr)-, (Cu, Cr)-3Si infiltration layer.In the case of simple 2Cr13 matrix,
Surface property is enhanced, but can be further enhanced by coating design performance, it is still further preferred that plating Cu, but Cu/Ni is compound simultaneously
It is not best.
Above the present invention is implemented provided to be only alloying Fe3It is wear-resisting, against corrosion comprehensive that Si infiltration layer improves 2Cr13 stainless steel
It closes the fused salt non-electrolytic preparation method of performance and what is carried out be discussed in detail, applies specific embodiment to the principle of the present invention in text
And embodiment is expounded, the above embodiments are only used to help understand, and method and its core of the invention is thought
Think, and can according to the thought of the present invention, in specific embodiments and applications for those of ordinary skill in the art
Adjustment can accordingly be changed, therefore the contents of this specification are not to be construed as limiting the invention.
Claims (10)
1. alloying Fe3Si infiltration layer improves the fused salt non-electrolytic preparation method of wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel, special
Sign is, carries out neutral fused salt siliconising preparation conjunction to the 2Cr13 matrix containing Cr alloying element or with coated 2Cr13 matrix
Aurification Fe3Si layers.
2. alloying Fe according to claim 13The fused salt that Si infiltration layer improves wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel is non-
Electrolytic preparation method, which is characterized in that prepare alloying Fe in neutral fused salt siliconising3Before Si layers, first 2Cr13 matrix is carried out
Pretreatment including two surface Mechanical Planarization, oil removing links, the surface 2Cr13 is smooth after processing, there is metallic luster, obtains
No greasy dirt, the attachment of non-corroding object and the metal surface without obvious oxide layer.
3. alloying Fe according to claim 13The fused salt that Si infiltration layer improves wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel is non-
Electrolytic preparation method, which is characterized in that prepare alloying Fe in neutral fused salt siliconising3Before Si layers, alloying source has been carried out
Design, that is, directly carry out neutral fused salt siliconising on 2Cr13 matrix, or prepare alloy by carrying out electro-deposition on the surface 2Cr13
The coat of metal needed for changing, then carries out neutral fused salt siliconising again.
4. alloying Fe according to claim 33The fused salt that Si infiltration layer improves wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel is non-
Electrolytic preparation method, which is characterized in that the metal coating material is Ni or/and Cu.
5. according to the alloying Fe of claim 3 or 43Si infiltration layer improves the molten of wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel
Salt non-electrolytic preparation method, which is characterized in that the thickness of coating is 5~20 μm, and coating is firmly combined with substrate, meets coating
Gross requirement.
6. according to claim 1 or the 3 alloying Fe3Si infiltration layer improves the molten of wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel
Salt non-electrolytic preparation method, which is characterized in that the fused salt is by neutral salt NaCl, KCl, NaF and siliconizing medium Na2Si6F, Si powder group
At 33%NaCl, 33%KCl, 14%NaF, 5%Na in molar ratio2SiF6, 15%Si configuration, carry out fused salt siliconising handle it
Before, neutral salt is dried into 1h at 100 DEG C, then be uniformly mixed with siliconizing medium and be ground into fine powder.
7. according to claim 1 or the 3 alloying Fe3Si infiltration layer improves the molten of wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel
Salt non-electrolytic preparation method, which is characterized in that in alloying Fe3In Si layers of preparation process, the 2Cr13 for designing alloy source is tried
Sample is embedded in the fused salt mixt in alumina crucible, it is ensured that specimen surface and fused salt fine powder come into full contact with, and quartz pushrod is also vertical
It is placed in fused salt, to stablize the source Si penetration enhancer.
8. alloying Fe according to claim 73The fused salt that Si infiltration layer improves wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel is non-
Electrolytic preparation method, which is characterized in that in alloying Fe3In Si layers of preparation process, 700~830 DEG C of holding temperature are set, heat preservation
2~4h of time.
9. alloying Fe according to claim 73The fused salt that Si infiltration layer improves wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel is non-
Electrolytic preparation method, which is characterized in that the alloy source is matrix or/and alloy source coating.
10. alloying Fe according to claim 13The fused salt of Si infiltration layer raising wear-resisting, the against corrosion comprehensive performance of 2Cr13 stainless steel
Non-electrolytic preparation method, which is characterized in that alloying Fe3After the completion of Si layers of infiltration system, quickly quartz pushrod and 2Cr13 sample are taken
Out, 2Cr13 sample is placed in air after natural cooling, clean the residual salt for removing surface repeatedly with hot water, and with acetone and nothing
Water-ethanol cleaning, dehydration and drying.
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| CN110993231A (en) * | 2019-11-25 | 2020-04-10 | 合肥工业大学 | Surface-alloyed high-corrosion-resistance sintered NdFeB magnet and preparation method thereof |
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| CN110408966B (en) * | 2019-09-04 | 2021-03-26 | 西安建筑科技大学 | Diffusion synthesis of nickel alloyed Fe3Method for enhancing comprehensive performance of steel surface by Si composite layer |
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