CN114875354A - High-strength seamless deformed steel and processing technology thereof - Google Patents

High-strength seamless deformed steel and processing technology thereof Download PDF

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CN114875354A
CN114875354A CN202210483109.XA CN202210483109A CN114875354A CN 114875354 A CN114875354 A CN 114875354A CN 202210483109 A CN202210483109 A CN 202210483109A CN 114875354 A CN114875354 A CN 114875354A
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deformed steel
sputtering
layer
permeation
nitriding
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CN114875354B (en
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吴小虎
吴志超
王啸桐
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Changzhou City Fangzheng Sectional Steel Co ltd
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Changzhou City Fangzheng Sectional Steel Co ltd
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    • 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
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    • 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
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    • C22C38/58—Ferrous alloys, e.g. steel alloys containing chromium with nickel with more than 1.5% by weight of manganese
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    • 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
    • C23C14/0021—Reactive sputtering or evaporation
    • C23C14/0036—Reactive sputtering
    • 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
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • 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
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0641—Nitrides
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    • 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
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    • 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
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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    • 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
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Abstract

The invention discloses a high-strength seamless deformed steel and a processing technology thereof, the scheme 316 austenitic stainless steel is used as a deformed steel matrix for processing, and the deformed steel comprises the following specific components: by mass fraction, 0.08% of C, 1% of Si, 2% of Mn, 0.35% of P, 0.03% of S, 10-14% of Ni, 16-18.5% of Cr, 2-3% of Mo and the balance of Fe; the deformed steel has higher strength and mechanical property. The scheme is characterized in that nitriding, co-infiltration and magnetron sputtering are carried out on the surface of the deformed steel, the whole process is reasonable in design, the operation is simple, the prepared deformed steel has excellent surface wear resistance, the strength is high, the surface hardness is high, the deformed steel can be widely applied to the technical fields of various building constructions, equipment processing and the like, and the method has high practicability.

Description

High-strength seamless deformed steel and processing technology thereof
Technical Field
The invention relates to the technical field of deformed steel, in particular to high-strength seamless deformed steel and a processing technology thereof.
Background
The deformed steel is a short for complicated and deformed section steel, belongs to one type of section steel, and is different from the calling method of the simple section steel. According to different processes, the steel can be divided into hot-rolled deformed steel, cold-drawn (cold-drawn) deformed steel, cold-bent deformed steel, welded deformed steel and the like. In general, the deformed steel is in particular hot-rolled deformed steel. The hot-rolled deformed steel is hot-rolled section steel which distinguishes square steel, round steel, flat steel and common shapes.
With the wider application of the deformed steel, the existing enterprises develop the production process of the deformed steel more and more deeply, and the performance requirements of the deformed steel are higher and higher, but the deformed steel produced by the prior art obviously cannot meet the requirements of people on the surface hardness and the wear resistance.
Based on the situation, the application discloses high-strength seamless deformed steel and a processing technology thereof, and aims to solve the technical problem.
Disclosure of Invention
The invention aims to provide high-strength seamless deformed steel and a processing technology thereof so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel;
(2) taking the deformed steel subjected to shot blasting, and performing ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding is performed for 4-5 hours at 520-530 ℃ to form a nitriding layer;
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, co-permeation is carried out for 3-4 hours at 530-540 ℃, a co-permeation layer is formed, and the pre-treated deformed steel is obtained by washing and drying with deionized water;
(3) taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 20-25 min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-penetration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 10-20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20-30 min;
and then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer for 1-1.5 hours by using a chromium target and aluminum palladium as sputtering sources, removing the mask after the sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially cleaning by using absolute ethyl alcohol and deionized water, and drying in vacuum to obtain a finished product.
According to an optimized scheme, in the step (1), the process parameters of shot blasting are as follows: the spraying pressure is 110-120 MPa, the spraying target distance is 20-30 mm, the nozzle moving speed is 400-450 mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 30-40 min.
According to an optimized scheme, in the step (2), nitriding process parameters are as follows: the cathode voltage is 600-700V, the nitrogen flow is 80-100 ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
in the optimized scheme, in the step (2), the co-permeation process parameters are as follows: the ammonia flow is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
According to the optimized scheme, in the step (3), an external magnetic field is introduced when the chromium nitride layer and the chromium aluminum nitride layer are sputtered, the direction of the external magnetic field is perpendicular to the pretreated deformed steel, and the intensity of the external magnetic field is 30-50 mT.
According to an optimized scheme, in the step (3), the pattern of the mask is formed by periodically arranging a plurality of hollow regular hexagons, the side length of each hollow regular hexagon is 20-30 μm, the hollow regular hexagons are spaced by spacers on the mask, and the width of each spacer is 10-15 μm.
In the more optimized scheme, in the step (3), the process parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 6-8 sccm, the flow rate of argon is 15-20 sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
In the optimized scheme, in the step (3), the technological parameters of the chromium aluminum nitride layer are as follows: the nitrogen flow is 6-8 sccm, the argon flow is 15-20 sccm, the chromium target power is 250W, the aluminum palladium power is 200-250W, and the cavity pressure is 0.5 Pa.
According to an optimized scheme, the deformed steel comprises the following components: the alloy comprises, by mass, 0.08% of C, 1% of Si, 2% of Mn, 0.35% of P, 0.03% of S, 10-14% of Ni, 16-18.5% of Cr, 2-3% of Mo and the balance of Fe.
According to an optimized scheme, the high-strength seamless deformed steel is prepared by the processing technology of the high-strength seamless deformed steel.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a high-strength seamless deformed steel and a processing technology thereof, the scheme 316 austenitic stainless steel is used as a deformed steel matrix for processing, and the deformed steel comprises the following specific components: by mass fraction, 0.08% of C, 1% of Si, 2% of Mn, 0.35% of P, 0.03% of S, 10-14% of Ni, 16-18.5% of Cr, 2-3% of Mo and the balance of Fe; the deformed steel has higher strength and mechanical property.
During this scheme adds man-hour earlier arrange deformed steel ultrasonic cleaning in acetone solution in, recycle anhydrous alcohol and deionized water and wash to get rid of its surface greasy dirt, carry out peening to it again, this peening's purpose is: the subsequent steps can carry out ion nitriding and ion co-infiltration treatment, after the surface of the deformed steel is subjected to shot blasting treatment, the co-infiltration layer is more continuous and compact during ion co-infiltration, the thickness of the co-infiltration layer is deeper, the quality of the co-infiltration layer is higher, and the bonding performance of the subsequent co-infiltration layer and the sputtering layer with the deformed steel is relatively more excellent.
After shot blasting treatment, ion nitriding is firstly carried out on the surface of the deformed steel, and the volume ratio of nitrogen to hydrogen is limited to 1: 4', the nitriding treatment is performed on the surface of the deformed steel, because: after nitriding treatment, the ferromagnetism of the surface of the deformed steel can be enhanced, when the deformed steel is matched with a subsequent external magnetic field, the magnetron sputtering effect can be improved, and a film layer formed by sputtering is more smooth and compact; meanwhile, after the surface nitriding treatment of the deformed steel, the surface hardness and the wear resistance of the deformed steel can be improved.
After surface nitriding treatment, the scheme is to perform ion co-permeation on the surface of a nitriding layer, catalyze the permeation by titanium sponge, and limit the co-permeation gas to be ethanol and carbon disulfide, wherein the volume ratio of the ethanol to the carbon disulfide is 4: 1', wherein carbon elements provided by ethanol and carbon disulfide can promote nitrogen diffusion, and introduction of sulfur elements can improve the wear resistance of the surface of the deformed steel; therefore, after the ion co-cementation is carried out, the surface hardness and the depth of a cementation layer are greatly improved, and the wear resistance and the corrosion resistance of the deformed steel are further improved.
Here, it is to be noted that: according to the scheme, nitriding and ion co-permeation treatment can be performed firstly, on one hand, the surface hardness of the deformed steel is improved, and on the other hand, the nitriding layer and the co-permeation layer can be used as a composite transition layer, so that subsequent deformed steel surface pattern design and corrosion-resistant sputtering film layer processing are facilitated.
On the basis of the scheme, firstly, carrying out chromium nitride layer on the surface of the deformed steel, controlling the sputtering time to be 10-20 min, fixing a mask plate on the surface of the deformed steel, continuously sputtering the chromium nitride layer, then, sputtering chromium nitride aluminum layers on the surface of the chromium nitride layer by taking a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1-1.5 h, a plurality of regularly arranged regular hexagonal patterns are formed on the surface of the deformed steel, grooves exist among the regular hexagonal patterns, the grooves are caused by the existence of the partition bars of the mask plate, and after the partition bars are removed, the chromium nitride layer and the chromium nitride aluminum layers are sputtered in the hollow regular hexagonal patterns of the mask plate; the spacers of the mask block sputtering, a groove can be formed after the mask is removed, and the bottom of the groove is the chromium nitride layer sputtered for the first time; due to the existence of the mask, in order to integrally ensure the corrosion resistance of the surface of the deformed steel, the chromium nitride layer is sputtered twice; meanwhile, the pattern arrangement on the surface of the deformed steel is also used for improving the surface wear resistance and reducing the surface wear.
The invention discloses high-strength seamless deformed steel and a processing technology thereof, the process design is reasonable, the operation is simple, the prepared deformed steel has excellent surface wear resistance, the strength is high, the surface hardness is high, the high-strength seamless deformed steel can be widely applied to the technical fields of various building constructions, equipment processing and the like, and the high-strength seamless deformed steel has high practicability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In this embodiment, the deformed steel is 316 austenitic stainless steel, and specifically comprises the following components: the alloy comprises, by mass, 0.08% of C, 1% of Si, 2% of Mn, 0.35% of P, 0.03% of S, 10-14% of Ni, 16-18.5% of Cr, 2-3% of Mo and the balance of Fe.
The pattern of the mask is formed by periodically arranging a plurality of hollow regular hexagons, the side length of each hollow regular hexagon is 25 mu m, the hollow regular hexagons are spaced by spacers on the mask, and the width of each spacer is 10 mu m.
Example 1:
a processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 110MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 30 min.
(2) Taking the deformed steel after shot blasting, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 520 ℃ for 5 hours to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 80ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, carrying out co-permeation for 4 hours at 530 ℃, forming a co-permeation layer, washing with deionized water, and drying to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 20min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 10 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 30 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 200W, and the pressure of the cavity is 0.5 Pa.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Example 2:
a processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 115MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 35 min.
(2) Taking the deformed steel after shot blasting, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 525 ℃ for 4.5h to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 90ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-cementation treatment on the surface of the nitriding layer in an ammonia environment, catalyzing the nitriding with titanium sponge, carrying out co-cementation for 3.5h at 535 ℃ by using a co-cementation gas which is a mixed gas of ethanol and carbon disulfide, forming a co-cementation layer, washing with deionized water, and drying to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 15 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 25 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
Then, a chromium target and aluminum palladium are used as sputtering sources, a chromium nitride aluminum layer is sputtered on the surface of the chromium nitride layer, the sputtering time is 1.2h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Example 3:
a processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 120MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 40 min.
(2) Taking the deformed steel after shot blasting treatment, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 530 ℃ for 4 hours to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 100ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, and co-permeation is carried out for 3 hours at 540 ℃ to form a co-permeation layer, and washing and drying with deionized water to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1.5h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Example 4: example 4 is a modification of example 3, in which example 4 introduces an externally applied magnetic field with a field strength of 30 mT.
A processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 120MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 40 min.
(2) Taking the deformed steel after shot blasting treatment, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 530 ℃ for 4 hours to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 100ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, and co-permeation is carried out for 3 hours at 540 ℃ to form a co-permeation layer, and washing and drying with deionized water to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1.5h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
When the chromium nitride layer and the chromium nitride aluminum layer are sputtered, an external magnetic field is introduced, the direction of the external magnetic field is vertical to the pretreated deformed steel, and the external magnetic field intensity is 30 mT.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Example 5: example 5 is a modification of example 3, in which example 5 introduces an externally applied magnetic field with a field strength of 50 mT.
A processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 120MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 40 min.
(2) Taking the deformed steel after shot blasting treatment, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 530 ℃ for 4 hours to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 100ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, and co-permeation is carried out for 3 hours at 540 ℃ to form a co-permeation layer, and washing and drying with deionized water to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1.5h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
When the chromium nitride layer and the chromium nitride aluminum layer are sputtered, an external magnetic field is introduced, the direction of the external magnetic field is vertical to the pretreated deformed steel, and the intensity of the external magnetic field is 50 mT.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Comparative example 1: comparative example 1 a control test was carried out on the basis of example 4, in comparative example 1 no mask was introduced.
A processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 120MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 40 min.
(2) Taking the deformed steel after shot blasting treatment, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 530 ℃ for 4 hours to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 100ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, and co-permeation is carried out for 3 hours at 540 ℃ to form a co-permeation layer, and washing and drying with deionized water to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 40 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1.5h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
When the chromium nitride layer and the chromium nitride aluminum layer are sputtered, an external magnetic field is introduced, the direction of the external magnetic field is vertical to the pretreated deformed steel, and the external magnetic field intensity is 30 mT.
And after the sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Comparative example 2: comparative example 2 a control test was conducted on the basis of example 4, and no nitriding treatment was conducted in comparative example 2.
A processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 120MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 40 min.
(2) Taking the special-shaped steel after shot blasting, carrying out co-permeation treatment on the surface of the special-shaped steel in an ammonia environment, accelerating permeation of titanium sponge, carrying out co-permeation for 3 hours at 540 ℃ by using co-permeation gas which is mixed gas of ethanol and carbon disulfide, forming a co-permeation layer, washing with deionized water, and drying to obtain the pretreated special-shaped steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources, wherein the sputtering time is 1.5h, and the technological parameters of the chromium nitride aluminum layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the chromium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
When the chromium nitride layer and the chromium nitride aluminum layer are sputtered, an external magnetic field is introduced, the direction of the external magnetic field is vertical to the pretreated deformed steel, and the external magnetic field intensity is 30 mT.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Comparative example 3: comparative example 3 a comparative experiment was carried out on the basis of example 4, in which comparative example 3 the chromium aluminium nitride layer was replaced by a titanium aluminium nitride layer.
A processing technology of high-strength seamless deformed steel comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel; the process parameters of the shot blasting treatment are as follows: the spraying pressure is 120MPa, the spraying target distance is 20mm, the nozzle moving speed is 400mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 40 min.
(2) Taking the deformed steel after shot blasting treatment, carrying out ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding at 530 ℃ for 4 hours to form a nitriding layer; the nitriding process parameters are as follows: the cathode voltage is 600V, the nitrogen flow is 100ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, and co-permeation is carried out for 3 hours at 540 ℃ to form a co-permeation layer, and washing and drying with deionized water to obtain the pretreated deformed steel; the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
(3) Taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 25min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20 min; the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 15sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
And then sputtering a titanium aluminum nitride layer on the surface of the chromium nitride layer by using a chromium target and aluminum palladium as sputtering sources for 1.5h, wherein the process parameters of the titanium aluminum nitride layer are as follows: the flow rate of nitrogen is 8sccm, the flow rate of argon is 20sccm, the power of the titanium target is 250W, the power of aluminum and palladium is 250W, and the pressure of the cavity is 0.5 Pa.
When the chromium nitride layer and the titanium aluminum nitride layer are sputtered, an external magnetic field is introduced, the direction of the external magnetic field is vertical to the pretreated deformed steel, and the external magnetic field intensity is 30 mT.
And removing the mask after sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially adopting absolute ethyl alcohol and deionized water for cleaning, and performing vacuum drying to obtain a finished product.
Detection experiment:
1. the surface hardness of the shaped steel samples prepared in examples 1 to 5 and comparative examples 1 to 3 was measured by a Vickers hardness tester model HV-1000, and 3 to 5 positions were measured and averaged and recorded.
2. The special-shaped steel samples prepared in examples 1-5 and comparative examples 1-3 are taken, surface wear resistance detection is carried out, a friction pair is an alumina ceramic ball (the diameter is 9.38mm), the friction mode is a circumference, the circumference radius is 5mm, the normal loading load is 4N, the special-shaped steel is ground at the rotating speed of 60r/min for 30min, and the wear rate is measured and calculated. The test temperature was 25 ℃ and 500 ℃.
3. Taking the special-shaped steel samples prepared in the examples 1-5 and the comparative examples 1-3, and carrying out a salt spray corrosion test according to the ASTM B117-97 standard, wherein the test temperature is 35 ℃, the test temperature is 5% of neutral NaCl solution, and the pH value is 6.5-7.2; and testing for 360h, and observing the surface corrosion condition.
Watch 1
Figure BDA0003628336040000121
Watch two
Figure BDA0003628336040000122
And (4) conclusion: the invention discloses high-strength seamless deformed steel and a processing technology thereof, the process design is reasonable, the operation is simple, the prepared deformed steel has excellent surface wear resistance, the strength is high, the surface hardness is high, the high-strength seamless deformed steel can be widely applied to the technical fields of various building constructions, equipment processing and the like, and the high-strength seamless deformed steel has high practicability.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A processing technology of high-strength seamless deformed steel is characterized by comprising the following steps: the method comprises the following steps:
(1) taking deformed steel, placing the deformed steel in an acetone solution for ultrasonic cleaning, then sequentially adopting absolute ethyl alcohol and deionized water for ultrasonic cleaning, and drying in vacuum; shot blasting is carried out on the surface of the deformed steel;
(2) taking the deformed steel subjected to shot blasting, and performing ion nitriding on the surface of the deformed steel, wherein nitriding gas is mixed gas of nitrogen and hydrogen, and nitriding is performed for 4-5 hours at 520-530 ℃ to form a nitriding layer;
carrying out co-permeation treatment on the surface of a nitriding layer in an ammonia environment, accelerating permeation of titanium sponge, wherein co-permeation gas is mixed gas of ethanol and carbon disulfide, co-permeation is carried out for 3-4 hours at 530-540 ℃, a co-permeation layer is formed, and the pre-treated deformed steel is obtained by washing and drying with deionized water;
(3) taking the pretreated deformed steel, transferring the deformed steel to vacuum, bombarding and cleaning the deformed steel for 20-25 min by argon, introducing nitrogen, sputtering a chromium nitride layer on the surface of the co-infiltration layer by taking a chromium target as a sputtering source, wherein the sputtering time is 10-20 min; fixing a mask plate on the surface of the pretreated deformed steel, and continuously sputtering a chromium nitride layer on the surface of the pretreated deformed steel fixed with the mask plate for 20-30 min;
and then sputtering a chromium nitride aluminum layer on the surface of the chromium nitride layer for 1-1.5 hours by using a chromium target and aluminum palladium as sputtering sources, removing the mask after the sputtering is finished, placing the pretreated deformed steel in an acetone solution for ultrasonic cleaning, sequentially cleaning by using absolute ethyl alcohol and deionized water, and drying in vacuum to obtain a finished product.
2. A process according to claim 1, wherein the process comprises the following steps: in the step (1), the process parameters of shot blasting are as follows: the spraying pressure is 110-120 MPa, the spraying target distance is 20-30 mm, the nozzle moving speed is 400-450 mm/min, the shot blasting is 304 stainless steel shot with the diameter of 0.5mm, and the spraying time is 30-40 min.
3. A process according to claim 1, wherein the process comprises the following steps: in the step (2), the nitriding process parameters are as follows: the cathode voltage is 600-700V, the nitrogen flow is 80-100 ml/min, the pressure in the furnace is 500Pa, and the volume ratio of the nitrogen to the hydrogen is 1: 4.
4. a process according to claim 1, wherein the process comprises the following steps: in the step (2), the co-permeation process parameters are as follows: the flow rate of ammonia gas is 2L/min, and the volume ratio of ethanol to carbon disulfide is 4: 1; the flow rate of the co-permeation gas was 0.2L/min.
5. A process according to claim 1, wherein the process comprises the following steps: in the step (3), an external magnetic field is introduced when the chromium nitride layer and the chromium nitride aluminum layer are sputtered, the direction of the external magnetic field is perpendicular to the pretreated deformed steel, and the intensity of the external magnetic field is 30-50 mT.
6. A process according to claim 1, wherein the process comprises the following steps: in the step (3), the pattern of the mask is formed by periodically arranging a plurality of hollow regular hexagons, the side length of each hollow regular hexagon is 20-30 μm, the hollow regular hexagons are spaced by spacers on the mask, and the width of each spacer is 10-15 μm.
7. A process according to claim 1, wherein the process comprises the following steps: in the step (3), the technological parameters of the chromium nitride layer are as follows: the flow rate of nitrogen is 6-8 sccm, the flow rate of argon is 15-20 sccm, the power of the chromium target is 100W, and the pressure of the cavity is 0.5 Pa.
8. A process according to claim 1, wherein the process comprises the following steps: in the step (3), the technological parameters of the chromium nitride aluminum layer are as follows: the nitrogen flow is 6-8 sccm, the argon flow is 15-20 sccm, the chromium target power is 250W, the aluminum palladium power is 200-250W, and the cavity pressure is 0.5 Pa.
9. A process according to claim 1, wherein the process comprises the following steps: the deformed steel comprises the following components: the alloy comprises, by mass, 0.08% of C, 1% of Si, 2% of Mn, 0.35% of P, 0.03% of S, 10-14% of Ni, 16-18.5% of Cr, 2-3% of Mo and the balance of Fe.
10. A high-strength seamless deformed steel produced by the process according to any one of claims 1 to 9.
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