CN106835055A - 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 PDFInfo
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- CN106835055A CN106835055A CN201710134695.6A CN201710134695A CN106835055A CN 106835055 A CN106835055 A CN 106835055A CN 201710134695 A CN201710134695 A CN 201710134695A CN 106835055 A CN106835055 A CN 106835055A
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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
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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
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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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
- 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
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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
- 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
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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
- 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, particularly a kind of nuclear grade stainless steel of wear resistant corrosion resistant, the surface treatment of the nuclear grade stainless steel includes note two steps of nitrogen and nitriding:The note nitrogen step is that 45 60KeV, implantation temperature controls in 300 400 DEG C, implantation dosage to be 6 × 10 in ion implantation energy17ions/cm2‑12×1017ions/cm2Under conditions of carry out;The nitridation steps in-furnace temperature be 450 490 DEG C, nitriding pressure be 280 330Pa, N2:H2 is 2.7:1‑3.3:1st, nitriding time be 15 19h, the 800V of ionization voltage 750, the 3.3A of ionization current 2.5 under conditions of carry out.By above-mentioned steps, a kind of bond strength can be formed on nuclear grade stainless steel surface high, corrosion resistance and good, wearability is far superior to the composite nitride layer of conventional Nitrizing Treatment, so as to significantly improve the combination property of nuclear grade stainless steel.
Description
Technical field
The present invention relates to technical field of metal material, more particularly to a kind of nuclear grade stainless steel of wear resistant corrosion resistant.
Background technology
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, hyperpyrexia
Stream, highly acid), most of parts because fretting wear can further corrosion and premature failure.
To improve its service life, it will usually which above-mentioned part is surface-treated, Nitrizing Treatment aiming at core level not
The more conventional means of rust steel.
Excessively thin nitration case cannot ensure the anti-wear performance of stainless steel at all, to obtain satisfied nitride thickness, generally
Need to carry out nitriding at relatively high temperatures, a large amount of precipitation of chromium causes matrix poor during high temperature nitriding can not only cause stainless steel base
Chromium, and it is not high with substrate combinating strength using the nitration case that high temperature nitriding is obtained, it is susceptible to peel off, once nitration case is shelled
Fall, chromium depleted matrix can be corroded in very short time, so as to cause part failure.
Research shows that Nitrizing Treatment is by many factors shadows such as material, temperature, atmosphere, voltage, electric current, time, the types of cooling
Ring, not yet form a complete theoretical system in the industry at present, technological parameter selection during practical application can without reliable rule
Follow, there is great blindness.
In view of the missing of ripe theoretical system, begin in recent years being surface-treated for nuclear grade stainless steel in this technology at present
Fail to obtain obvious breakthrough eventually.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of nuclear grade stainless steel of wear resistant corrosion resistant.
To achieve the above object, the present invention is adopted the following technical scheme that:
A kind of nuclear grade stainless steel of wear resistant corrosion resistant, it is characterised in that be surface-treated as follows:
Step one, note nitrogen:Ion implantation energy be 45-60KeV, implantation temperature control 300-400 DEG C, implantation dosage for 6 ×
1017ions/cm2-12×1017ions/cm2;
Glow discharge nitriding is carried out after step 2, note nitrogen:Nitriding temperature is 450-490 DEG C, and nitriding pressure is 250-330pa, N2:H2 is
2.7-3.3:1, nitriding time is 15-19h, and nitriding voltage is 750-800V, and electric current is 2.5-3.3A.
Preferably, before to nuclear grade stainless steel note nitrogen, its surface is pre-processed, process step includes:
1st, nuclear grade stainless steel is polished with 200#SiC silicon carbide papers, removes the cutting cut and greasy dirt on its surface, then used successively
400#, 600#, 800#, 1000# and 1200#SiC silicon carbide paper carry out mechanical grinding to workpiece surface;
2nd, its facet 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;
3rd, ultrasonic wave cleaning is carried out to workpiece in the mixed solution of acetone soln, distilled water and alcohol successively, when cleaning every time
Between be not less than 15 minutes.
Further, the ion implantation energy of the step one is 45KeV, and implantation temperature is 400 DEG C, and implantation dosage is 9
×1017ions/cm2-12×1017ions/cm2。
Further, the nitriding temperature of the step 2 is 480-490 DEG C, and nitriding time is 17h, and nitriding voltage is
800V, nitriding electric current is 3A.
Preferably, the nitriding temperature of the step one is 480 DEG C.
Preferably, the ion implantation energy of the step one be 45KeV, implantation temperature be 400 DEG C, implantation dosage be 9 ×
1017ions/cm2。
Compared with prior art, the invention has the advantages that:
1st, the nuclear grade stainless steel of the wear resistant corrosion resistant that the present invention is provided will note nitrogen and process as first surface process step, and will note
Nitrogen and Nitrizing Treatment are combined, and overcome the problem that nitriding is difficult to after note nitrogen, and the nuclear grade stainless steel for being obtained has good corrosion resistant concurrently
Corrosion and splendid wearability.
2nd, the wear resistant corrosion resistant nuclear grade stainless steel that the present invention is provided has the nitration case that nitrogen content is gradually changed, the nitration case
High with substrate combinating strength, up to 5Gpa effectively solves nitration case and is pressurized/impacts flaky problem.
3rd, wear resistant corrosion resistant nuclear grade stainless steel surface provided by the present invention forms the nitration case of different tissues structure, nitrogen
Change layer gross thickness and reach more than 100um, and nitridation layer surface forms single γ N phases, compared with individually note nitrogen/nitriding, its γ N phase
Broaden, intensity increases, the generation of γ N phases is conducive to the stainless steel after anti-corrosion resistance, therefore treatment in BAS with more
It is excellent corrosion resisting property.
4th, 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.
5th, the wear resistant corrosion resistant nuclear grade stainless steel that the present invention is provided, it is effective to reduce(Even avoid)High temperature nitriding is caused
Chromium separate out, maintain the excellent decay resistance of its matrix.
6th, the present invention provide wear resistant corrosion resistant nuclear grade stainless steel, without in traditional nitriding process because edge effect, surface rise
Nitration case that arc is caused is uneven and calcination phenomenon.
Brief description of the drawings
Fig. 1 is the nitride thickness microphoto of comparative example 2.
Fig. 2 is the nitride thickness microphoto of embodiment 3.
Fig. 3 is the cut of comparative example 2 test photo.
Fig. 4 is the cut of embodiment 3 test photo.
Fig. 5 is the electrochemical corrosion of comparative example 2 test photo.
Fig. 6 is the electrochemical corrosion of embodiment 3 test photo.
Fig. 7 is the vickers hardness test result of comparative example 2.
Fig. 8 is embodiment 3Wei Shi hardness test results.
Fig. 9 is the X-ray diffraction result of embodiment 3.
Specific embodiment
For the ease of the understanding of those skilled in the art, the present invention is made further with reference to embodiment and accompanying drawing
It is bright, it has to be noted that the content that following implementation methods are referred to not 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 to inject enhancing
Depositing device, LD-3 type ion-nitriding furnaces, drying box, the note nitrogen and nitriding that these equipment are commonly used for those skilled in the art set
Standby, test material used is core 304 stainless steels of level, chemical composition(In terms of mass fraction)For: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 surpluses.Specific preparation process is such as
Under:
The pretreatment of the first step, nuclear grade stainless steel
1)Polishing:With 200#SiC silicon carbide papers polish, remove surface cutting cut and greasy dirt, then successively with 400#,
600#, 800#, 1000# and 1200#SiC silicon carbide paper carry out mechanical grinding to nuclear grade stainless steel surface;
2)Polishing:Nylon polishing cloth and granularity are that 1.5 μm of diamond polishing cream is mechanically polished to each sample facet, table
Surface roughness reaches Ra≤0.05um;
3)Cleaning:Ultrasonic wave cleaning is carried out in the mixed solution of acetone soln, distilled water and alcohol successively, the time is about 15 points
Clock;
4)Dry:Nuclear grade stainless steel after cleaning is put such as cold air drying in drying box, is sealed stand-by.
Second step, nitrogen implantation:Set multifunction ion injection enhanced deposition is put into by the nuclear grade stainless steel of pretreatment
Standby to carry out note nitrogen, ion implantation energy is 45KV, implantation temperature is controlled at 300-400 DEG C, and implantation dosage is 6 × 1017ions/
cm2-12×1017ions/cm2;
3rd step, glow discharge nitriding:The nuclear grade stainless steel noted after nitrogen is put into carries out Nitrizing Treatment in ion-nitriding furnace, set in stove
Temperature is 450-490 DEG C, and nitriding pressure is 330pa, N2:H2It is 3:1, nitriding time is 15-19h.
The nuclear grade stainless steel surface treated using the above method can produce the uniform composite nitride layer of a layer thickness, the nitrogen
Changing layer has good wearability, corrosion resistance and the bond strength with matrix.Nitridation thickness >=the 100um, case hardness is remote
It is much better than existing glow discharge nitriding;XRD analysis display composite nitride layer possesses the γ N phases of single, wideization(Referring to), thus with good
Good corrosion resistance;Electrochemical corrosion test shows that the nuclear grade stainless steel corrosion potential after treatment is improved, 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 display composite nitride layer load is reachable
More than 60N, and scratching edge occurs without composite nitride layer peeling.
For the wear resistant corrosion resistant nuclear grade stainless steel that the checking present invention is provided notes nitrogen, nitrided surface handling process relative to existing
The improvement amplitude of the combination property of nuclear grade stainless steel afterwards, applicant has done 8 groups of examinations using existing process and above-mentioned preparation method
Test.Wherein, above-mentioned preparation method is totally five groups of embodiment 1-5;Nuclear grade stainless steel without any treatment is comparative example 1;By existing
There is technique to make Nitrizing Treatment for comparative example 2;Make note nitrogen by existing process and be processed as comparative example 3.
The difference of embodiment 1-5 essentially consists in and the partial parameters of second step and the 3rd step is adjusted, so that
Generate the slightly discrepant different nitration cases of property indices.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 measure of nitration case, vickers hardness test,
Electrochemical corrosion test, cut test(Measurement nitration case bond strength), test result is shown in Table 2.
Be can be seen that from upper table test result good comprehensive using being achieved to nuclear grade stainless steel of processing of the inventive method
Can, and considerably beyond traditional Nitrizing Treatment and the workpiece of nitrogen treatment is noted, it is necessary to be to above-mentioned result of the test special instruction, it is right
Ratio 3 is surface-treated using nitrogen injection method to nuclear grade stainless steel, although rate of corrosion is relatively low, but due to nitrogen injection method in itself
The characteristics of, its acquisition nitration case is very thin, so that it cannot carry out scratch test to test its bond strength, simultaneously because note nitrogen
Layer is thin, and wearability is poor, it is impossible to adapts to the harsh working environment of nuclear grade stainless steel, therefore generally will not will note nitrogen technique in the industry at present
For being surface-treated to nuclear power station control rod involucrum, process pipe, steam generator, pump, valve and cutter cutter hub.
Additionally, 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 contrast
The scratch test photo of example 2, Fig. 4 is embodiment scratch test photo, and Fig. 5 is the corrosion test photo of embodiment 3, and Fig. 6 is comparative example 2
Corrosion test photo)It can also be seen that uniform cross change of nitration case color shown in Fig. 2 from workpiece surface to junction, can
Seeing the nitration case has the gradient of nitrogen change in concentration, and above-mentioned graded is had no in Fig. 1;Comparison diagram 3 and Fig. 4, Fig. 3 again
Shown workpiece occurs in that edge Fragmentation Phenomena at cut, and this is apparently due to nitration case occurs in that peeling in test, and Fig. 4
There is not any peeling phenomenon at shown workpiece cut, show outstanding bond strength;Shown in comparison diagram 5 and Fig. 6, Fig. 5
Workpiece occurs in that obviously etch pit, and workpiece shown in Fig. 6 only occurs minor surface corrosion, and depth is not and matrix;It is right
It is far superior to workpiece shown in Fig. 7 than workpiece Vickers hardness shown in Fig. 7 and Fig. 8, Fig. 8, is answered considerably beyond nuclear grade stainless steel is actual
Hardness requirement.
Claims (7)
1. a kind of nuclear grade stainless steel of wear resistant corrosion resistant, is surface-treated using following methods:
Step one, note nitrogen:Ion implantation energy be 45-60KeV, implantation temperature control 300-400 DEG C, implantation dosage for 6 ×
1017ions/cm2-12×1017ions/cm2;
Glow discharge nitriding is carried out after step 2, note nitrogen:Nitriding temperature is 450-490 DEG C, nitriding pressure is 280-350Pa, N2:H2For
2.7:1-3.3:1st, nitriding time be 15-19h, nitriding voltage be 750-800V, nitriding electric current be 2.5-3.3A.
2. the nuclear grade stainless steel of wear resistant corrosion resistant according to claim 1, it is characterised in that carry out the note nitrogen step it
Before, first stainless steel surfaces are pre-processed, process step includes:
1), by pending nuclear grade stainless steel with 200#SiC silicon carbide papers polish, remove surface cutting cut and greasy dirt, then
Mechanical grinding is carried out to its surface with 400#, 600#, 800#, 1000# and 1200#SiC silicon carbide paper successively;
2), with the diamond polishing cream that nylon polishing cloth and granularity are 1.5 μm its buffed surface is mechanically polished, make its surface
Roughness reaches Ra≤0.05um;
3), ultrasonic wave cleaning is carried out in the mixed solution of acetone soln, distilled water and alcohol successively, every time cleaning time not
Less than 15 minutes.
3. the nuclear grade stainless steel of wear resistant corrosion resistant according to claim 2, it is characterised in that:The ion implanting of the step one
Energy is 45KeV, and implantation temperature is 400 DEG C, and implantation dosage is 9 × 1017ions/cm2-12×1017ions/cm2。
4. the nuclear grade stainless steel of wear resistant corrosion resistant according to claim 3, it is characterised in that:The nitriding temperature of the step 2
It it is 480-490 DEG C, nitriding time is 17h, nitriding voltage is 800V, and nitriding electric current is 3A.
5. according to claim 1-4 any one wear resistant corrosion resistant nuclear grade stainless steel, it is characterised in that:The step 2
Nitriding temperature be 480 DEG C.
6. according to claim 1-4 any one wear resistant corrosion resistant nuclear grade stainless steel, it is characterised in that:The step one
Ion implantation energy be 45KeV, implantation temperature be 400 DEG C, implantation dosage be 9 × 1017ions/cm2。
7. the nuclear grade stainless steel of wear resistant corrosion resistant according to claim 5, it is characterised in that:The ion implanting of the step one
Energy is 45KeV, and implantation temperature is 400 DEG C, and implantation dosage is 9 × 1017ions/cm2。
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