CN114107883B - Local ion nitriding method for inner cavity of precipitation hardening stainless steel annular part - Google Patents
Local ion nitriding method for inner cavity of precipitation hardening stainless steel annular part Download PDFInfo
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- CN114107883B CN114107883B CN202111433348.6A CN202111433348A CN114107883B CN 114107883 B CN114107883 B CN 114107883B CN 202111433348 A CN202111433348 A CN 202111433348A CN 114107883 B CN114107883 B CN 114107883B
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- seepage
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- 238000005121 nitriding Methods 0.000 title claims abstract description 75
- 229910001220 stainless steel Inorganic materials 0.000 title claims abstract description 45
- 239000010935 stainless steel Substances 0.000 title claims abstract description 45
- 238000004881 precipitation hardening Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000001105 regulatory effect Effects 0.000 claims abstract description 11
- 238000004321 preservation Methods 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 6
- 239000010406 cathode material Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 230000002265 prevention Effects 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 229910000963 austenitic stainless steel Inorganic materials 0.000 claims description 2
- 239000012459 cleaning agent Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims description 2
- 238000000576 coating method Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims 2
- 238000003754 machining Methods 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 8
- 238000009792 diffusion process Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910000734 martensite Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C23C8/04—Treatment of selected surface areas, e.g. using masks
Abstract
The invention relates to a method for local ion nitriding of an inner cavity of a 05Cr17Ni4Cu4Nb precipitation hardening stainless steel annular part. The anti-seepage tool comprises a designed anti-seepage tool, wherein the outer surface and the inner cavity of a part are protected without nitriding parts, the anti-seepage tool is placed in an ion nitriding furnace, nitriding gas is introduced, the gas flow is controlled, the electrical parameters in the nitriding process are regulated, the temperature in the furnace is increased to the required nitriding temperature, and the anti-seepage tool is slowly cooled after heat preservation is carried out at the nitriding temperature. According to the invention, the hardness and depth of the diffusion layer of the part to be nitrided in the 05Cr17Ni4Cu4Nb precipitation hardening stainless steel annular part meet the technical requirements, and the rest parts are free of nitriding layers under the protection of the tool; the hardness of the matrix is unchanged.
Description
Technical Field
The invention relates to the technical field of chemical heat treatment, in particular to a portable automatic on-line verification device for a feeler gauge.
Background
05Cr17Ni4Cu4Nb is a typical martensitic precipitation hardening stainless steel, and is aged to precipitate a precipitation hardening phase after solid solution and dispersed in a low-carbon martensitic matrix, so that the strength of the material is improved. Meanwhile, the material has excellent corrosion resistance and is widely applied to aerospace products.
The annular part uses 05Cr17Ni4Cu4Nb as a raw material, is used in a spherical unlocking device, and is a part for limiting a locking sleeve. After unlocking of the unlocking device, the locking sleeve will strike the spring cover part. In order to prevent damage to the contact surface, the contact surface is required to have a high hardness of 50HRC or more. And after the 05Cr17Ni4Cu4Nb precipitation hardening stainless steel is subjected to solid solution treatment and aging treatment, the highest hardness can only reach about 41-44 HRC, and the use requirement cannot be met. In order to improve the surface hardness of the part, an ion nitriding process is adopted, so that the service life of the part is prolonged. Meanwhile, in order to maintain the toughness of the matrix, the matrix hardness is required to be 28-32 HRC.
Ion nitriding is a chemical heat treatment method which utilizes a high-voltage electric field to decompose nitrogen-containing gas continuously introduced into a furnace, so that nitrogen plasma is generated to bombard the surface of a workpiece continuously to heat the workpiece, and active nitrogen atoms are generated to permeate the surface of the workpiece at the same time, so that the surface of the workpiece is reinforced. According to the method, local nitriding is carried out on the annular part with the complex inner cavity shape, the outer surface of the part and other parts of the inner cavity which do not need nitriding are required to be protected, the parts which do not need nitriding are prevented from being nitrided, and meanwhile, the nitriding effect of the parts which need nitriding of the inner cavity cannot be hindered by the protection tool. After nitriding is carried out by the method, the hardness of the part matrix is unchanged, the surface hardness of the part needing nitriding is more than or equal to HV1000, the depth of a permeation layer is more than or equal to 0.1mm, the permeation layer is uniform, and the effect that the part needing nitriding is free of the permeation layer is achieved.
Disclosure of Invention
The invention aims to provide a portable automatic on-line verification device for a feeler gauge, which protects the outer surface and the inner cavity of a part through tool design without nitriding parts, so that the part is free of a permeable layer. Adjusting temperature, time, electrical parameters and the like in the nitriding process, and determining proper technological parameters to ensure that the part of the inner cavity to be infiltrated meets the surface hardness proposed by the technical requirements
In order to solve the technical problems, the technical scheme of the invention is as follows: the method for locally nitriding the inner cavity of the precipitation hardening stainless steel annular part comprises the following steps:
s1, designing a tool: manufacturing an anti-seepage tool according to the size and shape of the precipitation hardening stainless steel part;
s2, preparation: cleaning precipitation hardening stainless steel parts and anti-seepage tools, and drying in an oven at the temperature of less than 100 ℃ or drying by using anhydrous oil-free compressed air;
s3, local protection: installing the seepage-proofing tool outside and at the bottom of the part;
s4, charging: uniformly placing a plurality of parts provided with the seepage-proofing tool on a cathode material tray in an annular shape;
s5, ion nitriding: nitriding the annular part.
Further, in the step S1, an anti-seepage tool is manufactured according to the size and shape of the precipitation hardening stainless steel part:
the precipitation hardening stainless steel part is in an annular structure; the inner cavity is provided with an annular protruding step, and the surface to be nitrided is an inner circular surface on the protruding step; the anti-seepage tool consists of a first component and a second component, wherein the first component covers the upper surface of the precipitation hardening stainless steel part, the middle through hole exposes the partial surface of the inner cavity which needs nitriding, and covers the part of the inner cavity which does not need nitriding; the second component is placed below the inner cavity of the precipitation hardening stainless steel part, a through hole is formed in the middle of the second component, the partial surface of the inner cavity needing nitriding is exposed, and the inner cavity is covered without nitriding parts.
Further, in the step S1, the anti-seepage tool is formed by processing 1Cr18Ni9 austenitic stainless steel.
In step S2, solvent type cleaning agents are applied to the inner and outer surfaces of the precipitation hardening stainless steel parts and the seepage prevention tool to clean surface dirt and oil stains, and the surfaces are dried in an oven at a temperature less than 100 ℃ or dried by anhydrous oil-free compressed air, so that the surfaces are ensured to be clean and dry.
Furthermore, in step S3, the first component of the anti-seepage tool covers the outside of the precipitation hardening stainless steel part, and the second component is placed at the bottom of the precipitation hardening stainless steel part, so that the outer surface and the inside of the precipitation hardening stainless steel part are completely covered without nitriding, and the part of the precipitation hardening stainless steel part, which needs nitriding, is exposed.
Further, in the step S4, the axial direction of the anti-seepage tooling is parallel to the axial direction of the cathode tray; the same gap of 20 mm-30 mm is kept between the tools and is positioned on the same circumference, and the gap between the tools and the furnace wall is 50 mm-60 mm.
Further, the step S5 includes:
s51: vacuumizing the ion nitriding furnace;
s52: igniting glow to clean the surface of the part by glow discharge;
s53: ammonia is introduced in the heating process, and the temperature is kept at the nitriding temperature;
s54: and after the heat preservation is finished, cooling and discharging.
Further, in the step S51, after the ion nitriding furnace is vacuumized, the vacuum degree is less than 50Pa; gradually increasing the voltage to ignite the glow in S52, wherein the voltage is not higher than 400V;
in S53, ammonia is introduced after the temperature rises to 400 ℃ at a heating rate of less than or equal to 200 ℃/h, and the flow rate of the ammonia is 3L/min-5L/min; then the temperature is increased to 560 ℃ at the speed of less than or equal to 120 ℃/h, and the temperature is kept for 10h. The pressure in the furnace is regulated to 300-500 Pa through a vacuum proportional valve, the regulating voltage is regulated to 400-800V, and the temperature is kept stable;
s54, furnace cooling is carried out after the heat preservation is finished, and ammonia gas is stopped being introduced after the furnace cooling is carried out to below 400 ℃; and cooling the furnace to below 70 ℃, taking out the anti-seepage tooling for coating the annular part, and dismantling the anti-seepage tooling to finish nitriding treatment.
Furthermore, the surface hardness of the part to be nitrided of the precipitation hardening stainless steel annular part subjected to ion nitriding is more than or equal to HV1000, and the depth of a permeation layer is more than or equal to 0.1mm.
Further, the hardness of the base body of the precipitation hardening stainless steel annular part subjected to ion nitriding is consistent with the hardness before nitriding.
The local ion nitriding method for the inner cavity of the precipitation hardening stainless steel annular part provided by the invention ensures that the hardness and depth of a permeation layer of a part needing nitriding in the 05Cr17Ni4Cu4Nb precipitation hardening stainless steel annular part meet the technical requirements, and the other parts do not have nitriding layers under the protection of a tool; the hardness of the matrix is unchanged.
Drawings
The invention is further described below with reference to the accompanying drawings:
FIG. 1 is a flow chart of a method of local ion nitriding of an inner cavity of a 05CrNi4Cu4Nb precipitation hardening stainless steel annular part of the present invention;
FIG. 2 is a schematic view of a precipitation-hardenable stainless steel annular part of the present invention;
FIG. 3 is a schematic view of a nitriding tool according to the present invention;
FIG. 4 is a schematic illustration of placement of a nitriding tool with parts on a cathode disk;
FIG. 5 is a photograph of a metallographic image of the present invention.
Detailed Description
The method for locally ion nitriding the inner cavity of the precipitation hardening stainless steel annular part according to the invention is further described in detail below with reference to the accompanying drawings and the specific examples. Advantages and features of the invention will become more apparent from the following description and from the claims. It is noted that the drawings are in a very simplified form and utilize non-precise ratios, and are intended to facilitate a convenient, clear, description of the embodiments of the invention.
Example 1:
referring to fig. 1-4, the method comprises the following steps:
step S1, described in detail below:
and manufacturing an anti-seepage tool (2) according to the size and shape of the precipitation hardening stainless steel annular part (1). The shape of the part is an annular structure; the inner cavity is provided with an annular protruding step, and the surface to be nitrided is an inner circular surface (11) on the protruding step. The anti-seepage tool (2) consists of a component (21) and a component (22), wherein the component (21) covers the upper surface of a part, a middle through hole is formed in the middle, the local surface of an inner cavity needing nitriding is exposed, and the part of the inner cavity needing nitriding is covered; the assembly (22) is placed below the inner cavity of the part, a through hole is formed in the middle of the assembly, the partial surface of the inner cavity needing nitriding is exposed, and the part of the inner cavity needing nitriding is covered.
And S2, cleaning the part (1) and the seepage-proofing tool (2), and drying in an oven with the temperature less than 100 ℃.
And S3, installing the anti-seepage tool outside and at the bottom of the part. Wherein the component (21) covers the outside of the part (1), and the component (22) is arranged at the bottom of the part (1). The method realizes that the outer surface and the inner part of the annular part (1) are not required to be completely covered by nitriding, and the nitriding part of the inner cavity of the annular part is exposed.
And S4, opening a release valve, opening a furnace door, and placing a plurality of parts provided with the seepage-proofing tool on the cathode material tray. The axial direction of the tooling is parallel to the axial direction of the cathode material tray; the same gap of 30mm is kept between the tools and the gap between the tools and the furnace wall is 60mm. Closing the furnace door and closing the air release valve.
Step S5, which includes steps S51 to S54, is specifically described as follows:
s51, turning on a vacuum pump, and vacuumizing until the pressure in the hearth is 50Pa;
s52, gradually increasing voltage (not higher than 400V) to ignite glow, and cleaning the surface of the part by utilizing glow discharge. When the surface of the part is not arcing, the cleaning is finished and the heating stage is started;
s53, after the temperature rises to 400 ℃ at the heating rate of 180 ℃/h, introducing ammonia gas, wherein the flow rate of the ammonia gas is 3L/min. Raising the temperature to 560 ℃ at the speed of 80 ℃/h, and preserving the heat for 10h; regulating the pressure in the furnace to be (400-500) Pa, regulating the voltage to be (700-800) V through a vacuum proportional valve, and keeping the temperature stable;
and S54, after the heat preservation is finished, gradually reducing the ammonia gas proportional valve, regulating the vacuum proportional valve, regulating the voltage, cooling the furnace to 400 ℃ at the speed of 120 ℃/h, stopping introducing ammonia gas, continuing cooling the furnace to 70 ℃ and discharging the furnace.
The surface hardness of the obtained local nitriding part is detected by adopting a micro Vickers hardness tester, and the depth and uniformity of a permeation layer are detected by adopting a metallographic method. The surface hardness of the seepage layer reaches (1019-1028) HV, the depth of the seepage layer is (0.123-0.124) mm, the design requirements are met, and the seepage layer is uniform. The hardness of the matrix is (280-288) HV, and is consistent with that of the matrix before nitriding.
What is not described in detail in this specification is prior art known to those skilled in the art. It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (5)
1. A local ion nitriding method for an inner cavity of a precipitation hardening stainless steel annular part is characterized by comprising the following steps:
s1, designing a tool: manufacturing an anti-seepage tool according to the size and shape of the precipitation hardening stainless steel part;
s2, preparation: cleaning precipitation hardening stainless steel parts and anti-seepage tools, and drying in an oven at the temperature of less than 100 ℃ or drying by using anhydrous oil-free compressed air;
s3, local protection: installing the seepage-proofing tool outside and at the bottom of the part;
s4, charging: uniformly placing a plurality of parts provided with the seepage-proofing tool on a cathode material tray in an annular shape;
s5, ion nitriding: nitriding the annular part;
in the step S1, manufacturing an anti-seepage tool according to the size and the shape of the precipitation hardening stainless steel part:
the precipitation hardening stainless steel part is in an annular structure; the inner cavity is provided with an annular protruding step, and the surface to be nitrided is an inner circular surface on the protruding step; the anti-seepage tool consists of a first component and a second component, wherein the first component covers the upper surface of the precipitation hardening stainless steel part, the middle through hole exposes the partial surface of the inner cavity which needs nitriding, and covers the outer surface of the part and the part which does not need nitriding above the nitriding surface of the inner cavity; the second component is arranged below the inner cavity of the precipitation hardening stainless steel part, a through hole is arranged in the middle of the second component, the partial surface of the inner cavity needing nitriding is exposed, and the part which does not need nitriding below the nitriding surface of the inner cavity is covered;
in the step S2, solvent cleaning agents are applied to the inner and outer surfaces of the precipitation hardening stainless steel part and the seepage prevention tool to clean surface dirt and oil stains, and the precipitation hardening stainless steel part and the seepage prevention tool are dried in an oven at the temperature of less than 100 ℃ or dried by anhydrous oilless compressed air, so that the surface is ensured to be clean and dry;
in the step S4, the axial directions of the seepage-proofing tool are parallel to the axial direction of the cathode material tray; the same gap of 20 mm-30 mm is kept between the tools and is positioned on the same circumference, and the gap between the tools and the furnace wall is 50 mm-60 mm;
the step S5 includes:
s51: vacuumizing the ion nitriding furnace;
s52: igniting glow to clean the surface of the part by glow discharge;
s53: ammonia is introduced in the heating process, and the temperature is kept at the nitriding temperature;
s54: cooling and discharging after heat preservation is finished;
in the step S51, after the ion nitriding furnace is vacuumized, the vacuum degree is less than 50Pa; gradually increasing the voltage to ignite the glow in S52, wherein the voltage is not higher than 400V;
in S53, ammonia is introduced after the temperature rises to 400 ℃ at a heating rate of less than or equal to 200 ℃/h, and the flow rate of the ammonia is 3L/min-5L/min; then raising the temperature to 560 ℃ at the speed of less than or equal to 120 ℃/h, and preserving the heat for 10h; the pressure in the furnace is regulated to 300 Pa-500 Pa through a vacuum proportional valve, the regulating voltage is regulated to 400V-800V, and the temperature is kept stable;
s54, furnace cooling is carried out after heat preservation is finished, and ammonia gas is stopped being introduced after cooling to below 400 ℃; and cooling the furnace to below 70 ℃, taking out the anti-seepage tooling for coating the annular part, and dismantling the anti-seepage tooling to finish nitriding treatment.
2. The method of ion nitriding a portion of an inner cavity of a precipitation hardening stainless steel annular part according to claim 1, wherein in step S1, the impermeable tooling is formed by machining 1Cr18Ni9 austenitic stainless steel.
3. The method for local ion nitriding of the inner cavity of a precipitation hardening stainless steel annular part according to claim 1, wherein in the step S3, the first component of the seepage prevention tool covers the outside of the precipitation hardening stainless steel part, and the second component is placed at the bottom of the precipitation hardening stainless steel part, so that the outer surface and the inside of the precipitation hardening stainless steel part are completely covered without nitriding, and the part, which needs nitriding, of the inside of the precipitation hardening stainless steel part is exposed.
4. The method for locally ion nitriding an inner cavity of a precipitation hardening stainless steel annular part according to claim 1, wherein the surface hardness of the part to be nitrided of the precipitation hardening stainless steel annular part after ion nitriding is equal to or more than HV1000, and the depth of a permeation layer is equal to or more than 0.1mm.
5. The method for localized ion nitriding of an inner cavity of a precipitation hardened stainless steel annular part according to claim 4, wherein the precipitation hardened stainless steel annular part after ion nitriding is performed, and the hardness of the base body is kept consistent with the hardness before nitriding.
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