CN115612972A - Steel surface layer thickness controllable nitrogen-containing martensite composite modified layer and process method thereof - Google Patents
Steel surface layer thickness controllable nitrogen-containing martensite composite modified layer and process method thereof Download PDFInfo
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- CN115612972A CN115612972A CN202211179362.2A CN202211179362A CN115612972A CN 115612972 A CN115612972 A CN 115612972A CN 202211179362 A CN202211179362 A CN 202211179362A CN 115612972 A CN115612972 A CN 115612972A
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- 239000010410 layer Substances 0.000 title claims abstract description 170
- 229910000734 martensite Inorganic materials 0.000 title claims abstract description 74
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 34
- 239000010959 steel Substances 0.000 title claims abstract description 34
- 239000002344 surface layer Substances 0.000 title claims abstract description 23
- 230000008569 process Effects 0.000 title claims abstract description 20
- 150000004767 nitrides Chemical class 0.000 claims abstract description 50
- 238000005121 nitriding Methods 0.000 claims abstract description 29
- 230000003647 oxidation Effects 0.000 claims abstract description 27
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 238000005496 tempering Methods 0.000 claims description 21
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 12
- 238000004140 cleaning Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 238000013020 steam cleaning Methods 0.000 claims description 6
- 238000010407 vacuum cleaning Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 3
- 238000000354 decomposition reaction Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 230000007797 corrosion Effects 0.000 abstract description 13
- 238000005260 corrosion Methods 0.000 abstract description 13
- 239000011159 matrix material Substances 0.000 abstract description 10
- 238000003860 storage Methods 0.000 abstract description 5
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- 229910001209 Low-carbon steel Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000005255 carburizing Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
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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
- C23C8/02—Pretreatment of the material to be coated
-
- 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
- C21D6/00—Heat treatment of ferrous alloys
-
- 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
- C23C8/10—Oxidising
- C23C8/16—Oxidising using oxygen-containing compounds, e.g. water, carbon dioxide
- C23C8/18—Oxidising 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
- C23C8/08—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
- C23C8/80—After-treatment
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F17/00—Multi-step processes for surface treatment of metallic material involving at least one process provided for in class C23 and at least one process covered by subclass C21D or C22F or class C25
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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
- C21D2211/00—Microstructure comprising significant phases
- C21D2211/008—Martensite
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- Organic Chemistry (AREA)
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- Crystallography & Structural Chemistry (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The invention discloses a nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness and a process method thereof. The invention designs a composite structure layer with high mechanical property and high corrosion resistance on the surface of the low-carbon alloy steel, then obtains a nitrogen-containing martensite, nitride and surface oxide composite modified layer with controllable layer thickness from inside to outside by utilizing the technologies of soft nitriding and steam oxidation, provides high hardness and excellent wear resistance and corrosion resistance by utilizing a nitrogen-containing fine-grained martensite supporting layer with the layer thickness of about 20-30 mu m and a high-nitrogen-content gradient nitride layer, slows down the corrosion of a matrix by utilizing the oil storage effect of a surface compact oxide and improves the corrosion resistance of the composite layer. The invention obtains the uniform composite structure modified layer with controllable layer thickness, and has excellent wear resistance and corrosion resistance.
Description
Technical Field
The invention relates to a nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness and a process method thereof, belonging to the technical field of surface treatment.
Background
Low carbon steel and low carbon alloy steel are used as main structural materials, have the characteristics of simple manufacturing process, excellent comprehensive performance, low cost and the like, and are widely used for manufacturing new energy vehicle transmission parts, mechanical structure parts, aerospace parts and the like. But because the low-carbon steel and the low-carbon alloy steel have low carbon element and alloy content and insufficient surface wear resistance and corrosion resistance, the service life of the product is greatly shortened, and the cost of replacement, maintenance and the like is increased. In order to improve the surface performance of the material, common carburizing, nitriding and soft nitriding surface modification processes can be carried out on the material. But the carburizing temperature is high, the influence on a matrix is large, a nitriding layer is shallow and is easy to peel off from the matrix, the depth of a hardened layer of the conventional soft nitriding support compound is shallow, and the performance of a modified layer is single, so that the requirements of service performance cannot be met. Therefore, the development of the related technology of the composite structure modified layer with excellent surface wear resistance and corrosion resistance of the low-carbon steel and the low-carbon alloy steel is urgently needed.
Disclosure of Invention
The invention aims to overcome the technical defects in the prior art and solve the technical problems, and relates to a nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness and a process method thereof, which are convenient to apply in the aspects of corrosion resistance and friction and wear resistance, in particular to the application of wear resistance and corrosion resistance on related parts for a coupler or an electronic clutch for a new energy vehicle.
The invention specifically adopts the following technical scheme: controllable nitrogen-containing martensite composite modified layer of steel surface layer thickness, including the base member, the surface of base member is provided with the nitride layer, the base member with be provided with nitrogen-containing martensite layer between the nitride layer, the surface of nitride layer is provided with the oxide layer.
In a preferred embodiment, the thickness of the oxide layer is 2 to 3 μm; the thickness of the nitride layer and the thickness of the nitrogen-containing martensite layer are both 20-22 mu m.
The invention also provides a process method of the nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness, which comprises the following steps:
step SS1: pre-cleaning the substrate;
step SS2: carrying out nitriding heat treatment on the substrate obtained by cleaning in the step SS1 to prepare a semi-formed substrate containing a nitrogen martensite layer and a nitride layer;
and step SS3: and (3) carrying out oxidation treatment on the semi-formed substrate obtained in the step SS2 to prepare a composite modified layer containing an oxide layer.
As a preferred embodiment, the step SS1 specifically includes: and (3) washing the base body by using a washing machine, then carrying out vacuum cleaning on the base body by using a vacuum soaking cleaning machine, then carrying out steam cleaning on the base body by using steam, and finally carrying out spraying treatment on the base body.
As a preferred embodiment, the temperature of the vacuum cleaning is 100-140 ℃; the steam cleaning time is 5-10 min, the spraying medium is A-78L hydrocarbon liquid, and the spraying time is 20s.
As a preferred embodiment, the step SS2 specifically includes:
step SS21: carrying out pre-oxidation treatment on the substrate cleaned in the step SS1 by using a tempering furnace;
step SS22: carrying out soft nitriding treatment on the substrate subjected to the pre-oxidation treatment by using a gas nitriding furnace, wherein the cooling process after the soft nitriding treatment comprises the following steps: the oil cooling medium 809XV cools the oil, and the oil is cooled for 20min and then cooled by air;
step SS23: and (3) tempering the substrate after the soft nitriding treatment by using a tempering furnace, wherein the tempering heat preservation temperature is 250 ℃, and air cooling is performed after tempering for 90min to obtain the semi-formed substrate containing the nitrogen martensite layer and the nitride layer.
As a preferred embodiment, the pre-oxidation treatment temperature is 370-390 ℃, and the pre-oxidation treatment time is 40-50 min.
In a preferred embodiment, the soft-nitriding conditions are: the treatment temperature is 580-650 ℃, the treatment time is 150-180min 2 The speed is 30-50L/min, NH 3 The rate is 180-200L/min, CO 2 The speed is 0-6L/min, and the ammonia decomposition rate is 45-70%.
As a preferred embodiment, the tempering temperature is 220-250 ℃, and the tempering time is 60-80 min.
As a preferred embodiment, the step SS3 specifically includes: and (3) carrying out oxidation treatment on the semi-formed substrate containing the nitrogen martensite layer and the nitride layer obtained in the step SS2, wherein the oxidation treatment conditions are as follows: the oxidation temperature is 500-540 ℃, the oxidation time is 100-140 min, and the distilled water flow is 35-45 mL/h.
The invention achieves the following beneficial effects: firstly, compared with the traditional soft nitriding process, the invention designs a component and performance gradient change layer, and shows excellent effects in the aspects of comprehensive mechanical property and corrosion resistance. Secondly, the nitrogen-containing cryptocrystal martensite layer with ideal comprehensive mechanical properties is used as a middle supporting layer, so that the nitride layer and the substrate can be connected in a transition layer manner, the nitride hardened layer is prevented from being peeled off from the substrate, and the high hardness and the high wear resistance of the nitride layer can be ensured by virtue of higher hardness. The oxide with uniform and compact surface is used for isolating corrosive medium, and the capillary oil storage function of the micropores is used for obviously slowing down the corrosion of the matrix and improving the corrosion resistance of the composite layer.
Drawings
FIG. 1 is a schematic structural diagram of an embodiment 1 of the nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness according to the invention;
FIG. 2 is a cross-sectional view of the steel surface layer thickness controllable nitrogen-containing martensite composite modified layer of the embodiment 2 of the present invention, from the outside to the inside, an oxide layer, a nitride layer and a nitrogen-containing martensite layer are respectively shown, the oxide layer is about 2-3 μm, and the thickness of the nitride layer and the thickness of the nitrogen-containing martensite layer are both controlled at about 20 μm;
FIG. 3 is the microscopic morphology of the oxide layer, the nitride layer and the nitrogen-containing martensite layer after the amplification of the embodiment 2 of the present invention, and it can be seen from the figure that the oxide layer is straight and uniform, the interface transition bonding of the nitride layer and the nitrogen-containing martensite layer is good, and the martensite layer is uniformly and finely cryptocrystalline martensite;
FIG. 4 is a schematic diagram of energy spectrum analysis of different selected regions in the composite modified layer of example 2 of the present invention;
FIG. 5 is a graph of a power spectrum analysis of the nitride layer of spectrum 1 in FIG. 4;
FIG. 6 is a graph of a spectral analysis of the nitrogen-containing martensite layer of spectrum 2 in FIG. 4;
FIG. 7 is a graph of a spectrum analysis of the matrix of spectrum 3 in FIG. 4; it can be seen from the graph that the nitrogen content in the nitride layer, the nitrogen-containing martensite layer and the matrix are obviously different;
FIG. 8 is a cross-sectional nitrogen content scanning curve of the composite modified layer, from which it can be seen that the nitrogen content gradually decreases from the outside to the inside;
FIG. 9 is a photograph of the topography of the surface oxide, from which it can be seen that the oxide is uniformly dense;
FIG. 10 is an XRD analysis pattern of the composite modified layer, and the analysis result in combination with FIG. 4 indicates that the surface oxide is Fe 3 O 4 Nitrides mainly of Fe 3 N is formed;
FIG. 11 is a cross-sectional view of a nitrogen-containing martensite composite modified layer with a controllable layer thickness on the steel surface of example 3 of the present invention, in which a nitride layer and a nitrogen-containing martensite layer are respectively seen from the outside to the inside, and the thickness of the nitride layer and the thickness of the nitrogen-containing martensite layer are larger than those of example 1, and the structure is relatively coarse;
FIG. 12 is a cross-sectional view of a nitrogen-containing martensite composite modified layer with a controllable layer thickness on the steel surface of example 4 of the present invention, in which a nitride layer and a nitrogen-containing martensite layer are respectively seen from the outside to the inside, the layer thickness of the nitride layer is larger than that of example 1, and the structure is relatively coarse;
FIG. 13 is a cross-sectional view showing the surface layer of a steel substrate obtained in comparative example 1 of the present invention at a soft-nitriding temperature of 560 ℃ from the outside to the inside, showing a nitride layer and a substrate, respectively, showing no martensite layer, and having a surface hardness of 530 to 525HV0.1.
The meanings of the symbols in the figures: 1-substrate, 2-nitrogen-containing martensite layer, 3-nitride layer and 4-oxide layer.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1: as shown in figure 1, the invention provides a nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness, which comprises a base body 1, wherein a nitride layer 3 is arranged on the outer surface of the base body 1, a nitrogen-containing martensite layer 2 is arranged between the base body 1 and the nitride layer 3, and an oxide layer 4 is arranged on the outer surface of the nitride layer 3.
In a preferred embodiment, the thickness of the oxide layer 4 is 2 to 3 μm; the thickness of the nitride layer 3 and the thickness of the nitrogen-containing martensite layer 2 are both 20-22 μm.
Example 2: the invention also provides a process method of the nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness, which comprises the following 3 steps.
Step SS1: pre-cleaning the substrate; washing the base body with water by using a washing machine (model is BCA-1000), then carrying out vacuum cleaning on the base body by using a vacuum soaking cleaning machine (model is HWBV-4V-1000), then carrying out steam cleaning on the base body by using steam, and finally carrying out spraying treatment on the base body; the temperature of the vacuum cleaning is 100 ℃; the steam cleaning time is 5min, the spraying treatment medium is A-78L hydrocarbon liquid, and the spraying time is 20s.
Step SS2: carrying out nitriding heat treatment on the substrate obtained by cleaning in the step SS1 to prepare a semi-formed substrate containing a nitrogen martensite layer and a nitride layer; the method specifically comprises the following steps: step SS21: carrying out pre-oxidation treatment on the substrate cleaned in the step SS1 by adopting a tempering furnace with the model number of BTF-1000; step SS22: carrying out soft nitriding treatment on the pre-oxidized matrix by adopting a gas nitriding furnace with the model number of UNB-1000The subsequent cooling process comprises the following steps: cooling the oil by adopting an oil cooling medium 809XV, cooling for 20min, and then cooling by air; step SS23: tempering the substrate subjected to the soft nitriding treatment by adopting a tempering furnace with the model of BTF-1000, wherein the tempering heat preservation is 250 ℃, and the semi-formed substrate containing a nitrogen martensite layer and a nitride layer is obtained by air cooling after tempering for 90 min; the pre-oxidation treatment temperature is 380 ℃, and the pre-oxidation treatment time is 40min; the soft nitriding treatment conditions are as follows: the treatment temperature is 580 ℃, the treatment time is 150min 2 At a rate of 30L/min, NH 3 Rate of 180L/min, CO 2 The speed is 3L/min, and the ammonia decomposition rate is 45 percent; the tempering temperature is 220 ℃, and the tempering time is 60min.
And step SS3: carrying out oxidation treatment on the semi-formed substrate obtained in the step SS2 to prepare a composite modified layer containing an oxide layer; the step SS3 specifically includes: and (3) carrying out oxidation treatment on the semi-formed substrate containing the nitrogen martensite layer and the nitride layer obtained in the step SS2, wherein the oxidation treatment conditions are as follows: the oxidation temperature is 500 ℃, the oxidation time is 100min, and the distilled water flow is 35mL/h.
FIG. 2 is a cross-sectional view of the nitrogen-containing martensite composite modified layer with controllable layer thickness on the steel surface, from the outside to the inside, an oxide layer, a nitride layer and a nitrogen-containing martensite layer are respectively seen, the oxide layer is about 2-3 μm, and the thickness of the nitride layer and the thickness of the nitrogen-containing martensite layer are both controlled at about 20 μm; FIG. 3 shows the micro-morphology of the oxide layer, the nitride layer and the nitrogen-containing martensite layer, from which it can be seen that the oxide layer is straight and uniform, the interface of the nitride layer and the nitrogen-containing martensite layer is well-combined, and there are no defects of cracks, peeling and the like, and the martensite layer is internally provided with uniform and fine cryptocrystal martensite.
The composite modified layer containing the oxide layer obtained above was subjected to a neutral salt spray test: the sample was placed in a 50g/L aqueous solution of sodium chloride at 35 ℃ in a volume of 80cm 2 The average sedimentation rate of the horizontal area of the steel plate is 1.1ml/h, and the surface does not have obvious corrosion phenomenon after 120 h.
FIG. 4 is a schematic diagram of energy spectrum analysis of different selected regions in the composite modified layer of example 2 of the present invention; FIG. 5 is a graph of a power spectrum analysis of the nitride layer of spectrum 1 in FIG. 4; FIG. 6 is a graph of a spectral analysis of the nitrogen-containing martensite layer of spectrum 2 in FIG. 4; FIG. 7 is a graph of a spectrum analysis of the matrix of spectrum 3 in FIG. 4; it can be seen from the following tables one, two and three that the nitrogen contents in the nitride layer, the nitrogen-containing martensite layer and the matrix are significantly different.
TABLE 1 Nitrogen content in the nitride layer
| Element(s) | wt％ | at％ |
| C | 3.97 | 13.86 |
| N | 6.31 | 18.85 |
| Fe | 89.72 | 67.29 |
| Total amount of | 100.00 | 100.00 |
TABLE II Nitrogen content in the Nitrogen-containing martensite layer
| Element(s) | wt％ | at％ |
| C | 5.28 | 18.63 |
| N | 4.21 | 12.72 |
| Fe | 90.51 | 68.65 |
| Total amount of | 100.00 | 100.00 |
TABLE III is the nitrogen content in the matrix
| Element(s) | wt％ | at％ |
| C | 5.34 | 19.91 |
| N | 1.73 | 5.52 |
| Fe | 92.93 | 74.57 |
| Total amount of | 100.00 | 100.00 |
The surface oxide layer in this example is mainly (ferroferric oxide) Fe 3 O 4 The nitrides consisting essentially of (Fe-III-N) Fe 3 N composition, (the results of the phase analysis have been confirmed by XRD analysis pattern 10).
Example 3: the temperature for soft nitriding in this example was 620 ℃ as in example 2. FIG. 11 is a cross-sectional view of the nitrogen-containing martensite composite modified layer with a controllable layer thickness on the steel surface of example 3 of the present invention, in which the nitride layer and the nitrogen-containing martensite layer are respectively seen from the outside to the inside, and the thickness of the nitride layer and the nitrogen-containing martensite layer is larger than that of example 1, and the structure is relatively coarse.
Example 4: the temperature for soft nitriding in this example was 650 ℃ as in example 2. FIG. 12 is a cross-sectional view of the nitrogen-containing martensite composite modified layer in which the layer thickness on the steel surface is controllable in example 4 of the present invention, and it can be seen that the layer thickness of the nitride layer is larger than that in example 1 and the martensite structure is relatively coarse, respectively, from the outside to the inside.
The hardness of the obtained nitrogen-containing martensite layer is shown in table four.
Watch four
Table four shows hardness values of three regions, A, B and C, between the near nitrided layer and the near substrate, respectively, in the nitrogen-containing martensitic layer of fig. 12 obtained in example 2, fig. 11 obtained in example 3 and example 4, and the regions A, B and C were measured using an FM-810 vickers hardness tester with a load of 0.98N and a dwell time of 15 s. From the hardness results, it is understood that the nitrogen-containing martensite having the soft nitriding temperature of 580 ℃ is relatively high in hardness as compared with those of 620 ℃ and 650 ℃ and that the martensite layer has a relatively uniform thickness structure.
Comparative example 1: the temperature of soft nitriding in this example was 560 ℃, as in example 2, and as shown in FIG. 13, the cross-sectional profile of the surface layer of the steel substrate obtained in comparative example 1 of the present invention using a temperature of soft nitriding of 560 ℃ was shown, in which the oxide layer, the nitride layer and the substrate were separated from the outside to the inside, no martensite layer was formed, and the surface hardness was 530 to 525HV0.1.
It should be noted that the present invention has been made with respect to the appearance, hardness, metallographic phase and thickness of the carburized layer according to the standard of gas nitrocarburizing for GB/T22560-2008 steel parts, and the accompanying figures 4, 11, 12 and 13 illustrating the present invention have unnecessary comments, which are included in the analytical test procedures and will help those skilled in the art to understand the analytical procedures.
As will be appreciated by one skilled in the art, embodiments of the present application may be provided as a method, system, or computer program product. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present application may take the form of a computer program product embodied on one or more computer-usable storage media (including, but not limited to, disk storage, CD-ROM, optical storage, and so forth) having computer-usable program code embodied therein.
The present application is described with reference to flowchart illustrations and/or block diagrams of methods, apparatus (systems), and computer program products according to embodiments of the application. It will be understood that each flow and/or block of the flow diagrams and/or block diagrams, and combinations of flows and/or blocks in the flow diagrams and/or block diagrams, can be implemented by computer program instructions. These computer program instructions may be provided to a processor of a general purpose computer, special purpose computer, embedded processor, or other programmable data processing apparatus to produce a machine, such that the instructions, which execute via the processor of the computer or other programmable data processing apparatus, create means for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks. These computer program instructions may also be stored in a computer-readable memory that can direct a computer or other programmable data processing apparatus to function in a particular manner, such that the instructions stored in the computer-readable memory produce an article of manufacture including instruction means which implement the function specified in the flowchart flow or flows and/or block diagram block or blocks. These computer program instructions may also be loaded onto a computer or other programmable data processing apparatus to cause a series of operational steps to be performed on the computer or other programmable apparatus to produce a computer implemented process such that the instructions which execute on the computer or other programmable apparatus provide steps for implementing the functions specified in the flowchart flow or flows and/or block diagram block or blocks.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.
Claims (10)
1. Controllable nitrogenous martensite composite modified layer of steel surface layer thickness, its characterized in that includes base member (1), the surface of base member (1) is provided with nitride layer (3), base member (1) with be provided with nitrogenous martensite layer (2) between nitride layer (3), the surface of nitride layer (3) is provided with oxide layer (4).
2. The nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness according to claim 1, wherein the thickness of the oxide layer (4) is 2-3 μm; the thickness of the nitride layer (3) and the thickness of the nitrogen-containing martensite layer (2) are both 20-22 mu m.
3. The process method for preparing the nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness according to claim 1 is characterized by comprising the following steps:
step SS1: pre-cleaning the substrate;
step SS2: carrying out nitriding heat treatment on the substrate obtained by cleaning in the step SS1 to prepare a semi-formed substrate containing a nitrogen martensite layer and a nitride layer;
and step SS3: and (3) carrying out oxidation treatment on the semi-formed substrate obtained in the step SS2 to prepare a composite modified layer containing an oxide layer.
4. The nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness according to claim 3, wherein the step SS1 specifically comprises: and (3) washing the base body by using a washing machine, then carrying out vacuum cleaning on the base body by using a vacuum soaking cleaning machine, then carrying out steam cleaning on the base body by using steam, and finally carrying out spraying treatment on the base body.
5. The process method for preparing the nitrogen-containing martensite composite modified layer with the controllable steel surface layer thickness according to claim 4, wherein the temperature for vacuum cleaning is 100-140 ℃; the steam cleaning time is 5-10 min, the spraying medium is A-78L hydrocarbon liquid, and the spraying time is 20s.
6. The process method for preparing the nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness according to claim 3, wherein the step SS2 specifically comprises the following steps:
step SS21: carrying out pre-oxidation treatment on the substrate cleaned in the step SS1 by using a tempering furnace;
step SS22: carrying out soft nitriding treatment on the substrate subjected to the pre-oxidation treatment by using a gas nitriding furnace, wherein the cooling process after the soft nitriding treatment comprises the following steps: cooling the oil by using an oil cooling medium 809XV, and cooling by air after cooling for 20 min;
step SS23: and (3) tempering the substrate after the soft nitriding treatment by using a tempering furnace, wherein the tempering heat preservation temperature is 250 ℃, and air cooling is performed after tempering for 90min to obtain the semi-formed substrate containing the nitrogen martensite layer and the nitride layer.
7. The process method for preparing the nitrogen-containing martensite composite modified layer with the controllable steel surface layer thickness according to claim 6, wherein the pre-oxidation treatment temperature is 370-390 ℃, and the pre-oxidation treatment time is 40-50 min.
8. The process method for preparing the nitrogen-containing martensite composite modified layer with the controllable steel surface layer thickness according to claim 6, wherein the soft nitriding treatment conditions are as follows: the treatment temperature is 580-650 ℃, the treatment time is 150-180min 2 The speed is 30-50L/min, NH 3 The rate is 180-200L/min, CO 2 The speed is 0-6L/min, and the ammonia decomposition rate is 45-70%.
9. The process method for preparing the nitrogen-containing martensite composite modified layer with the controllable steel surface layer thickness according to claim 6, wherein the tempering temperature is 220-250 ℃, and the tempering time is 60-80 min.
10. The process method for preparing the nitrogen-containing martensite composite modified layer with controllable steel surface layer thickness according to claim 3, wherein the step SS3 specifically comprises the following steps: and (3) carrying out oxidation treatment on the semi-formed substrate containing the nitrogen martensite layer and the nitride layer obtained in the step SS2, wherein the oxidation treatment conditions are as follows: the oxidation temperature is 500-540 ℃, the oxidation time is 100-140 min, and the distilled water flow is 35-45 mL/h.
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