CN106835055B - A kind of nuclear grade stainless steel of wear resistant corrosion resistant - Google Patents

A kind of nuclear grade stainless steel of wear resistant corrosion resistant Download PDF

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Publication number
CN106835055B
CN106835055B CN201710134695.6A CN201710134695A CN106835055B CN 106835055 B CN106835055 B CN 106835055B CN 201710134695 A CN201710134695 A CN 201710134695A CN 106835055 B CN106835055 B CN 106835055B
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stainless steel
nitriding
ions
grade stainless
wear resistant
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CN106835055A (en
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唐德文
邹树梁
任宇宏
邓话
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University of South China
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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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/48—Ion implantation
    • 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
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/08—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24—Nitriding
    • C23C8/26—Nitriding of ferrous surfaces
    • 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
    • C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
    • C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
    • C23C8/38—Treatment of ferrous surfaces

Abstract

The present invention relates to technical field of metal material, especially a kind of nuclear grade stainless steel of wear resistant corrosion resistant, the surface treatment of the nuclear grade stainless steel include note two steps of nitrogen and nitriding: the note nitrogen step is ion implantation energy is 45-60KeV, injection temperature control in 300-400 DEG C, implantation dosage is 6 × 1017ions/cm2‑12×1017ions/cm2Under conditions of carry out；The nitridation steps in-furnace temperature be 450-490 DEG C, nitriding pressure 280-330Pa, N2:H2 2.7:1-3.3:1, nitriding time 15-19h, ionization voltage 750-800V, ionization current 2.5-3.3A under conditions of carry out.Through the above steps, a kind of bond strength height can be formed on nuclear grade stainless steel surface, corrosion resistance and good, wearability is far superior to the composite nitride layer of conventional Nitrizing Treatment, to significantly improve the comprehensive performance of nuclear grade stainless steel.

Description

A kind of nuclear grade stainless steel of wear resistant corrosion resistant
Technical field
The present invention relates to technical field of metal material, in particular to a kind of nuclear grade stainless steel of wear resistant corrosion resistant.
Background technique
In nuclear power engineering application, austenitic stainless steel is widely used because its is nonmagnetic, such as makes control rod involucrum, Process pipe, steam generator, pump, valve and cutter cutter hub etc., right its Service Environment very severe (high temperature, high pressure, high fever Stream, highly acid), most of components can further corrode due to premature failure because of fretting wear.
To improve its service life, it will usually above-mentioned component is surface-treated, Nitrizing Treatment aiming at nuclear leve not The rust more common means of steel.
Excessively thin nitration case not can guarantee the wear-resisting property of stainless steel at all, to obtain satisfied nitride thickness, usually Need to carry out nitriding at relatively high temperatures, high temperature nitriding, which not only will lead to chromium in stainless steel base and largely be precipitated, causes matrix poor Chromium, and it is not high with substrate combinating strength using the nitration case that high temperature nitriding obtains, it is easy to happen peeling, once nitration case is shelled It falls, chromium depleted matrix can be corroded in a very short period of time, so as to cause part failure.
Studies have shown that Nitrizing Treatment is by many factors shadow such as material, temperature, atmosphere, voltage, electric current, time, type of cooling It rings, not yet forms a complete theoretical system in the industry at present, technological parameter selection when practical application can without reliable rule It follows, there are great blindness.
In view of the missing of mature theoretical system, it is surface-treated in this technology and begins in recent years for nuclear grade stainless steel at present Fail to obtain apparent breakthrough eventually.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of nuclear grade stainless steels of wear resistant corrosion resistant.
To achieve the above object, the present invention adopts the following technical scheme:
A kind of nuclear grade stainless steel of wear resistant corrosion resistant, which is characterized in that be surface-treated as follows:
Step 1: note nitrogen: ion implantation energy 45-60KeV, injection temperature control are in 300-400 DEG C, implantation dosage 6×1017ions/cm2-12×1017ions/cm2；
Step 2: carrying out glow discharge nitriding after note nitrogen: nitriding temperature is 450-490 DEG C, nitriding pressure 250-330pa, N2: H2 is 2.7-3.3:1, and nitriding time 15-19h, nitriding voltage is 750-800V, electric current 2.5-3.3A.
Preferably, before infusing nitrogen to nuclear grade stainless steel, its surface is pre-processed, processing step includes:
1, by nuclear grade stainless steel with 200#SiC silicon carbide paper polish, remove the cutting scratch and greasy dirt on its surface, then according to It is secondary that mechanical grinding is carried out to workpiece surface with 400#, 600#, 800#, 1000# and 1200#SiC silicon carbide paper；
2, its facet is mechanically polished with the diamond polishing cream that nylon polishing cloth and granularity are 1.5 μm, makes it Surface roughness reaches Ra≤0.05um；
3, ultrasonic cleaning successively is carried out to workpiece in the mixed solution of acetone soln, distilled water and alcohol, it is clear every time The time is washed not less than 15 minutes.
Further, the ion implantation energy of the step 1 is 45KeV, and injection temperature is 400 DEG C, implantation dosage 9 ×1017ions/cm2-12×1017ions/cm2。
Further, the nitriding temperature of the step 2 is 480-490 DEG C, nitriding time 17h, and nitriding voltage is 800V, nitriding electric current are 3A.
Preferably, the nitriding temperature of the step 1 is 480 DEG C.
Preferably, the ion implantation energy of the step 1 be 45KeV, injection temperature be 400 DEG C, implantation dosage be 9 × 1017ions/cm2。
Compared with prior art, the invention has the following advantages:
1, the nuclear grade stainless steel of wear resistant corrosion resistant provided by the invention will infuse nitrogen processing and be used as first surface processing step, and Nitrogen will be infused and Nitrizing Treatment combines, overcome the problem of being difficult to nitriding after infusing nitrogen, nuclear grade stainless steel obtained has both good Corrosion resistance and splendid wearability.
2, the nitration case that there is wear resistant corrosion resistant nuclear grade stainless steel provided by the invention nitrogen content to gradually change, the nitration case With substrate combinating strength height, up to 5Gpa, effective solution nitration case compression/flaky problem of impact.
3, wear resistant corrosion resistant nuclear grade stainless steel provided by the present invention surface forms the nitration case of different tissues structure, nitrogen Change layer overall thickness and reach 100um or more, and nitrogenizes layer surface and form single γ N phase, compared with individually note nitrogen/nitriding, γ N phase It broadens, intensity increases, and the generation of γ N phase is conducive to anti-corrosion resistance, therefore treated that stainless steel has more in boric acid solution For excellent corrosion resisting property.
4, the hardness of wear resistant corrosion resistant nuclear grade stainless steel provided by the present invention is obviously improved, and reaches as high as 1500HV0.1, Wearability obtains breakthrough raising.
5, wear resistant corrosion resistant nuclear grade stainless steel provided by the invention, effective (or even avoiding) high temperature nitriding that reduces cause Chromium be precipitated, maintain the excellent corrosion resistance of its matrix.
6, wear resistant corrosion resistant nuclear grade stainless steel provided by the invention, because edge effect, surface are risen in no traditional nitriding process Nitration case caused by arc is uneven and calcination phenomenon.
Detailed description of the invention
Fig. 1 is 2 nitride thickness microphoto of comparative example.
Fig. 2 is 3 nitride thickness microphoto of embodiment.
Fig. 3 is 2 scratch of comparative example test photo.
Fig. 4 is 3 scratch of embodiment test photo.
Fig. 5 is 2 electrochemical corrosion of comparative example test photo.
Fig. 6 is 3 electrochemical corrosion of embodiment test photo.
Fig. 7 is 2 vickers hardness test result of comparative example.
Fig. 8 is 3 vickers hardness test result of embodiment.
Fig. 9 is 3 X-ray diffraction result of embodiment.
Specific embodiment
For the ease of the understanding of those skilled in the art, the present invention is made further below with reference to embodiment and attached drawing It is bright, it has to be noted that the content that following embodiments refer to not is limitation of the invention.
The equipment that preparing wear resistant corrosion resistant nuclear grade stainless steel of the present invention need to use has multifunction ion injection enhancing Depositing device, LD-3 type ion-nitriding furnace, drying box, these equipment are that those skilled in the art commonly infuse nitrogen and nitriding is set Standby, test material used is 304 stainless steel of nuclear leve, chemical component (based on mass fraction) are as follows: C≤0.07%, Si≤1.0%, Mn ≤ 2.0%, Cr:17.0% ~ 19.0%, Ni:8.0% ~ 12.0%, P≤0.035%, S≤0.03%, Fe surplus.Specific preparation step is such as Under:
The pretreatment of the first step, nuclear grade stainless steel
1) polish: with 200#SiC silicon carbide paper polish, remove the cutting scratch and greasy dirt on surface, then successively with 400#, 600#, 800#, 1000# and 1200#SiC silicon carbide paper carry out mechanical grinding to nuclear grade stainless steel surface；
2) polish: the diamond polishing cream that nylon polishing cloth and granularity are 1.5 μm carries out mechanical throwing to each sample facet Light, surface roughness reach Ra≤0.05um；
3) it cleans: successively carrying out ultrasonic cleaning in the mixed solution of acetone soln, distilled water and alcohol, the time is about 15 minutes；
4) dry: the nuclear grade stainless steel after cleaning to be put such as cold air drying in drying box, sealing is stand-by.
Second step, nitrogen implantation: it will be put into multifunction ion injection enhanced deposition by pretreated nuclear grade stainless steel and set Standby to carry out note nitrogen, at 300-400 DEG C, implantation dosage is 6 × 10 for ion implantation energy 45KV, the control of injection temperature17ions/ cm2-12×1017ions/cm2；
Third step, glow discharge nitriding: the nuclear grade stainless steel after note nitrogen is put into ion-nitriding furnace and carries out Nitrizing Treatment, is arranged In-furnace temperature is 450-490 DEG C, nitriding pressure 330pa, N2:H2For 3:1, nitriding time 15-19h.
The uniform composite nitride layer of a layer thickness, the nitrogen can be generated using the processed nuclear grade stainless steel surface of the above method Changing layer has good wearability, corrosion resistance and the bond strength with matrix.Nitridation thickness >=the 100um, surface hardness are remote It is much better than existing glow discharge nitriding；XRD analysis shows that composite nitride layer has single, wideization γ N phase (referring to), thus has good Good corrosion resistance；Electrochemical corrosion test shows that treated, and nuclear grade stainless steel corrosion potential improves, and corrosion current increases Slowly, the nuclear grade stainless steel of the more traditional Nitrizing Treatment of rate of corrosion is greatly lowered；Scratch test shows that composite nitride layer load is reachable 60N or more, and scratching edge does not occur composite nitride layer peeling.
To verify wear resistant corrosion resistant nuclear grade stainless steel provided by the invention relative to existing note nitrogen, nitrided surface treatment process The improvement amplitude of the comprehensive performance of nuclear grade stainless steel afterwards, applicant have done 8 groups of examinations using prior art and above-mentioned preparation method It tests.Wherein, above-mentioned preparation method is totally five groups of embodiment 1-5；Nuclear grade stainless steel without any processing is comparative example 1；By existing Having technique to make Nitrizing Treatment is comparative example 2；Making note nitrogen processing by prior art is comparative example 3.
The difference of embodiment 1-5, which essentially consists in, adjusts the partial parameters of second step and third step, thus Produce the slightly discrepant different nitration cases of performance indexes.The specific processing parameter of each embodiment and comparative example see the table below 1 It is shown.
For above-described embodiment 1-5 and comparative example 1-3, applicant carried out the micro- thickness measures of nitration case, Vickers hardness Test, electrochemical corrosion test, scratch test (measurement nitration case bond strength), test result is shown in Table 2.
It can be seen that from upper table test result good comprehensive using being achieved to nuclear grade stainless steel for the method for the present invention processing Performance is closed, and considerably beyond the workpiece of traditional Nitrizing Treatment and note nitrogen processing, needs to illustrate above-mentioned test result It is that comparative example 3 is surface-treated nuclear grade stainless steel using nitrogen injection method, although rate of corrosion is lower, due to infusing nitrogen side The characteristics of method itself, it is very thin to obtain nitration case, so that it cannot scratch test is carried out to test its bond strength, while by Thin in note nitrogen layer, wearability is poor, can not adapt to the harsh working environment of nuclear grade stainless steel, therefore will not will usually infuse in the industry at present Nitrogen technique is used for nuclear power station control rod involucrum, process pipe, steam generator, and pump, valve and cutter cutter hub are surface-treated.
In addition, from Fig. 1-6, (Fig. 1 is the microphoto of comparative example 2, and Fig. 2 is the microphoto of embodiment 3, and Fig. 3 is comparison 2 scratch test photo of example, Fig. 4 are embodiment scratch test photos, and Fig. 5 is 3 corrosion test photo of embodiment, and Fig. 6 is comparative example 2 Corrosion test photo) it can also be seen that uniform cross variation of nitration case color shown in Fig. 2 from workpiece surface to junction, it can Seeing the nitration case has the gradient of nitrogen concentration variation, and above-mentioned change of gradient is had no in Fig. 1；Comparison diagram 3 and Fig. 4 again, Fig. 3 There is edge Fragmentation Phenomena at scratch in shown workpiece, this is apparently due to nitration case occurs peeling off in test, and Fig. 4 Do not occur any peeling phenomenon at shown workpiece scratch, shows outstanding bond strength;Comparison diagram 5 and Fig. 6, shown in Fig. 5 There is obviously etch pit in workpiece, and minor surface corrosion only occurs for workpiece shown in Fig. 6, and depth is not and matrix；It is right Than Fig. 7 and Fig. 8, workpiece Vickers hardness shown in Fig. 8 is far superior to workpiece shown in Fig. 7, answers considerably beyond nuclear grade stainless steel is practical Hardness requirement.

Claims (7)

1. a kind of 304 stainless steel of nuclear leve of wear resistant corrosion resistant, is surface-treated using following methods:
Step 1: note nitrogen: ion implantation energy 45-60KeV, the control of injection temperature 300-400 DEG C, implantation dosage be 6 × 1017ions/cm2-12×1017ions/cm2；
Step 2: carrying out glow discharge nitriding after note nitrogen: nitriding temperature is 450-490 DEG C, nitriding pressure 280-350Pa, N2:H2For 2.7:1-3.3:1, nitriding time 15-19h, nitriding voltage are 750-800V, nitriding electric current is 2.5-3.3A.
2. 304 stainless steel of nuclear leve of wear resistant corrosion resistant according to claim 1, which is characterized in that carry out the note nitrogen step Before rapid, first 304 stainless steel surface of nuclear leve is pre-processed, processing step includes:
1), 304 stainless steel of nuclear leve to be processed 200#SiC silicon carbide paper is polished, removes the cutting scratch and greasy dirt on surface, so Mechanical grinding successively is carried out to its surface with 400#, 600#, 800#, 1000# and 1200#SiC silicon carbide paper afterwards；
2), its buffed surface is mechanically polished with the diamond polishing cream that nylon polishing cloth and granularity are 1.5 μm, makes its surface Roughness reaches Ra≤0.05um；
3) ultrasonic cleaning, is successively carried out in the mixed solution of acetone soln, distilled water and alcohol, the time cleaned every time is not Lower than 15 minutes.
3. 304 stainless steel of nuclear leve of wear resistant corrosion resistant according to claim 2, it is characterised in that: the ion of the step 1 Implantation Energy is 45KeV, and injection temperature is 400 DEG C, and implantation dosage is 9 × 1017ions/cm2-12×1017ions/cm2。
4. 304 stainless steel of nuclear leve of wear resistant corrosion resistant according to claim 3, it is characterised in that: the nitriding of the step 2 Temperature is 480-490 DEG C, nitriding time 17h, and nitriding voltage is 800V, and nitriding electric current is 3A.
5. 304 stainless steel of nuclear leve of wear resistant corrosion resistant described in -4 any one according to claim 1, it is characterised in that: the step Rapid two nitriding temperature is 480 DEG C.
6. 304 stainless steel of nuclear leve of wear resistant corrosion resistant described in -4 any one according to claim 1, it is characterised in that: the step Rapid one ion implantation energy is 45KeV, and injection temperature is 400 DEG C, and implantation dosage is 9 × 1017ions/cm2。
7. 304 stainless steel of nuclear leve of wear resistant corrosion resistant according to claim 5, it is characterised in that: the ion of the step 1 Implantation Energy is 45KeV, and injection temperature is 400 DEG C, and implantation dosage is 9 × 1017ions/cm2。
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