CN118048601A - Ion nitriding composite surface modification treatment method - Google Patents

Ion nitriding composite surface modification treatment method Download PDF

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Publication number
CN118048601A
CN118048601A CN202410402784.4A CN202410402784A CN118048601A CN 118048601 A CN118048601 A CN 118048601A CN 202410402784 A CN202410402784 A CN 202410402784A CN 118048601 A CN118048601 A CN 118048601A
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stainless steel
parts
steel plate
ion nitriding
nitrogen
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景荣富
景翀翀
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Yuyao Jingyuan Heat Treatment Co ltd
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Yuyao Jingyuan Heat Treatment Co ltd
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/36Solid 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
    • C23C8/38Treatment of ferrous surfaces
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/07Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 containing phosphates
    • C23C22/08Orthophosphates
    • C23C22/12Orthophosphates containing zinc cations
    • C23C22/17Orthophosphates containing zinc cations containing also organic acids
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/02Pretreatment of the material to be coated
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C8/00Solid 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
    • C23C8/06Solid 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
    • C23C8/34Solid 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 more than one element being applied in more than one step
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19Iron or steel
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/06Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using emulsions

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  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

The invention discloses an ion nitriding composite surface modification treatment method, which comprises the following steps: cutting stainless steel plates: stainless steel sheet surface treatment: the method comprises the steps that a seepage promoting agent dripping device is arranged above a heating container, nitrogen is introduced into the heating container, the seepage promoting agent is dripped into the heating container through the seepage promoting agent dripping device, the temperature in the heating container is increased, so that the gaseous seepage promoting agent is mixed with the nitrogen, and the mixing ratio of the gaseous seepage promoting agent to the nitrogen is 1:4, a step of; and placing the stainless steel into a vacuum ion nitriding furnace, and adjusting the vacuum degree of the vacuum ion nitriding furnace to be 30-40Pa. According to the invention, after the stainless steel plate is cut, the stainless steel plate is subjected to oil removal, oxidation film removal and impurity removal, and the surface of the stainless steel plate is subjected to phosphating treatment, so that a porous and loose phosphating layer is formed on the surface of the stainless steel plate, and the diffusion and adsorption of active nitrogen atoms are promoted by mixing the gaseous permeation promoter with nitrogen, so that the ion nitriding efficiency is improved.

Description

Ion nitriding composite surface modification treatment method
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to an ion nitriding composite surface modification treatment method.
Background
Ion nitriding is a chemical heat treatment process in which a furnace body is used as an anode, a workpiece to be treated is used as a cathode, and hundreds of volts of direct current voltage is applied between the anode and the cathode to generate glow discharge for nitriding treatment in a low-vacuum nitrogen-containing atmosphere. Ion nitriding is known by various names such as ion nitriding, glow discharge nitriding, ion bombardment nitriding, plasma nitriding, and the like.
The ion nitriding is carried out in a vacuum chamber, a workpiece is connected with a negative electrode of a high-voltage direct-current power supply, a single positive electrode is connected in vacuum, the vacuum degree of the vacuum chamber is pumped to 10Pa, and a small amount of nitrogen or mixed gas of hydrogen and nitrogen is filled. When the voltage is regulated to 400-800V, nitrogen is ionized and decomposed into nitrogen ions, hydrogen ions and electrons, and glow discharge phenomenon is generated on the surface of the workpiece. The positive ions are accelerated to bombard the surface of the workpiece under the action of an electric field, so that the workpiece is heated to nitriding temperature, nitrogen ions obtain electrons on the surface of the steel part, are reduced to nitrogen atoms, permeate the surface of the steel part and diffuse into the steel part to form a nitriding layer.
However, at present, when stainless steel is nitrided, the nitriding efficiency is low, and the processing efficiency of the stainless steel is reduced to a certain extent.
Therefore, an ion nitriding composite surface modification treatment method is provided for the problems.
Disclosure of Invention
The invention aims to provide an ion nitriding composite surface modification treatment method, which comprises the following steps:
Step one: cutting stainless steel plates: selecting a stainless steel plate, cutting the stainless steel plate by using a laser cutting machine, and polishing the cut part of the stainless steel plate by using a mirror surface polisher;
Step two: stainless steel sheet surface treatment:
① . Deoiling: preparing a chemical degreasing agent, wherein the chemical degreasing agent comprises the following raw materials in parts by weight: 40-50 parts of sodium hydroxide, 10-20 parts of sodium phosphate, 10-20 parts of emulsifying agent, 1-5 parts of trisodium phosphate, 1-3 parts of triethanolamine and the balance of water, and sequentially placing the sodium hydroxide, the sodium phosphate, the emulsifying agent, the trisodium phosphate, the triethanolamine and the water in a stirrer, and uniformly stirring to obtain a chemical degreasing agent;
Soaking the stainless steel plate in a chemical degreasing agent for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
② . Acid-base composite treatment: soaking the deoiled stainless steel plate in a sodium hydroxide solution with the mass concentration of 1-3% for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying; soaking the stainless steel plate in 1-3% sulfuric acid for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
③ . Phosphating: preparing phosphating solution, wherein the phosphating solution comprises the following raw materials in parts by weight: 20-40 parts of phosphoric acid, 10-20 parts of nitric acid, 10-20 parts of zinc nitrate, 5-10 parts of citric acid, 1-3 parts of sodium dodecyl benzene sulfonate, 1-2 parts of octyl phenol polyoxyethylene ether and the balance of water, and sequentially placing the phosphoric acid, the nitric acid, the zinc nitrate, the citric acid, the sodium dodecyl benzene sulfonate, the octyl phenol polyoxyethylene ether and the water in a stirrer, and uniformly stirring to obtain phosphating solution;
soaking the stainless steel plate in phosphating solution, carrying out ultrasonic oscillation treatment for 1-2 hours, taking out the stainless steel plate, washing with deionized water, and drying;
Step three: mixing of gases: the method comprises the steps that a seepage promoting agent dripping device is arranged above a heating container, nitrogen is introduced into the heating container, the seepage promoting agent is dripped into the heating container through the seepage promoting agent dripping device, the temperature in the heating container is increased, so that the gaseous seepage promoting agent is mixed with the nitrogen, and the mixing ratio of the gaseous seepage promoting agent to the nitrogen is 1:4, a step of;
Step four: ion nitriding: putting stainless steel into a vacuum ion nitriding furnace, adjusting the vacuum degree of the vacuum ion nitriding furnace to be 30-40Pa, introducing helium gas to perform ion bombardment for 20-30min at the temperature of 300-350 ℃, stopping ion bombardment, and introducing mixed gas of a gaseous permeation promoter and nitrogen, wherein the mixing ratio of the mixed gas of ammonia and hydrogen is 1:1.5, heating the temperature in the nitriding furnace to 500-550 ℃, regulating the pressure in the vacuum nitriding furnace to 130-150Mpa, maintaining the treatment time for 4-6h, stopping introducing the mixed gas of the gaseous catalyst and nitrogen, introducing the mixed gas of ammonia and hydrogen into the vacuum ion nitriding furnace, increasing the pressure in the furnace to 150-200Mpa, and continuing for 1-2h to finish nitriding;
Step five: oxidation reaction: stopping introducing oxygen into the mixed gas of ammonia and hydrogen, continuously cooling to room temperature along with the furnace after the temperature in the vacuum nitriding furnace is reduced to 300-400 ℃ for 1-2h and stopping introducing oxygen after an oxide film is formed on the surface of stainless steel, and introducing ammonia after the temperature is reduced to 200-250 ℃.
Preferably, the ultrasonic power of the ultrasonic treatment in the second step is 1000W, and the frequency is 50kHz.
Compared with the prior art, the invention has the following beneficial effects:
According to the invention, after the stainless steel plate is cut, the operations of removing oil, removing oxidation films and removing impurities are carried out on the stainless steel plate, and phosphating treatment is carried out on the surface of the stainless steel plate, so that a porous and loose phosphating layer is formed on the surface of the stainless steel plate, and the diffusion and adsorption of active nitrogen atoms are promoted by mixing the gaseous permeation agent with nitrogen, so that the ion nitriding efficiency is improved, and after the ion nitriding is finished, the oxidation films are formed on the surface of the stainless steel plate by introducing oxygen, and the corrosion resistance of the stainless steel plate is improved.
Drawings
Fig. 1 is a flow chart of the method steps of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
As shown in the attached figure 1, the ion nitriding composite surface modification treatment method provided by the invention comprises the following steps:
Step one: cutting stainless steel plates: selecting a stainless steel plate, cutting the stainless steel plate by using a laser cutting machine, and polishing the cut part of the stainless steel plate by using a mirror surface polisher;
Step two: stainless steel sheet surface treatment:
① . Deoiling: preparing a chemical degreasing agent, wherein the chemical degreasing agent comprises the following raw materials in parts by weight: 40 parts of sodium hydroxide, 15 parts of sodium phosphate, 15 parts of emulsifying agent, 5 parts of trisodium phosphate, 3 parts of triethanolamine and the balance of water, and sequentially placing 40 parts of sodium hydroxide, 15 parts of sodium phosphate, 15 parts of emulsifying agent, 5 parts of trisodium phosphate, 3 parts of triethanolamine and 22 parts of water into a stirrer, and uniformly stirring to obtain a chemical degreasing agent;
Soaking the stainless steel plate in a chemical degreasing agent for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
② . Acid-base composite treatment: soaking the deoiled stainless steel plate in a sodium hydroxide solution with the mass concentration of 1-3% for 30min, performing ultrasonic treatment for 5min, taking out, cleaning with deionized water, and drying; then soaking the stainless steel plate in sulfuric acid with the mass concentration of 3% for 30min, carrying out ultrasonic treatment for 5min, taking out, cleaning with deionized water, and drying;
wherein, the ultrasonic power of ultrasonic treatment is 1000W, and the frequency is 50kHz;
③ . Phosphating: preparing phosphating solution, wherein the phosphating solution comprises the following raw materials in parts by weight: 40 parts of phosphoric acid, 15 parts of nitric acid, 15 parts of zinc nitrate, 10 parts of citric acid, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of octyl phenol polyoxyethylene ether and 15 parts of water are sequentially placed into a stirrer, and uniformly stirred to obtain phosphating solution;
soaking the stainless steel plate in phosphating solution, carrying out ultrasonic oscillation treatment for 1-2 hours, taking out the stainless steel plate, washing with deionized water, and drying;
Step three: mixing of gases: the method comprises the steps that a seepage promoting agent dripping device is arranged above a heating container, nitrogen is introduced into the heating container, the seepage promoting agent is dripped into the heating container through the seepage promoting agent dripping device, the temperature in the heating container is increased, so that the gaseous seepage promoting agent is mixed with the nitrogen, and the mixing ratio of the gaseous seepage promoting agent to the nitrogen is 1:4, a step of;
Step four: ion nitriding: putting stainless steel into a vacuum ion nitriding furnace, adjusting the vacuum degree of the vacuum ion nitriding furnace to 40Pa, introducing helium gas to perform ion bombardment for 30min at the temperature of 300 ℃, stopping ion bombardment, and introducing mixed gas of a gaseous permeation accelerator and nitrogen, wherein the mixing ratio of the mixed gas of ammonia and hydrogen is 1:1.5, heating the temperature in the nitriding furnace to 500 ℃, regulating the pressure in the vacuum nitriding furnace to 130Mpa, maintaining the treatment time for 6h, stopping introducing the mixed gas of the gaseous catalyst and nitrogen, introducing the mixed gas of ammonia and hydrogen into the vacuum ion nitriding furnace, increasing the pressure in the furnace to 150Mpa, and continuing for 2h to finish nitriding;
step five: oxidation reaction: stopping introducing oxygen into the mixed gas of ammonia and hydrogen, continuously cooling for 2 hours when the temperature in the vacuum nitriding furnace is reduced to 300 ℃, stopping introducing oxygen after an oxide film is formed on the surface of stainless steel, introducing ammonia, and cooling to room temperature along with the furnace after the temperature is reduced to 200 ℃.
Examples
An ion nitriding composite surface modification treatment method comprises the following steps:
Step one: cutting stainless steel plates: selecting a stainless steel plate, cutting the stainless steel plate by using a laser cutting machine, and polishing the cut part of the stainless steel plate by using a mirror surface polisher;
Step two: stainless steel sheet surface treatment:
① . Deoiling: preparing a chemical degreasing agent, wherein the chemical degreasing agent comprises the following raw materials in parts by weight: 40 parts of sodium hydroxide, 15 parts of sodium phosphate, 15 parts of emulsifying agent, 5 parts of trisodium phosphate, 3 parts of triethanolamine and the balance of water, and sequentially placing 40 parts of sodium hydroxide, 15 parts of sodium phosphate, 15 parts of emulsifying agent, 5 parts of trisodium phosphate, 3 parts of triethanolamine and 22 parts of water into a stirrer, and uniformly stirring to obtain a chemical degreasing agent;
Soaking the stainless steel plate in a chemical degreasing agent for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
② . Acid-base composite treatment: soaking the deoiled stainless steel plate in a sodium hydroxide solution with the mass concentration of 1-3% for 30min, performing ultrasonic treatment for 5min, taking out, cleaning with deionized water, and drying; then soaking the stainless steel plate in sulfuric acid with the mass concentration of 3% for 30min, carrying out ultrasonic treatment for 5min, taking out, cleaning with deionized water, and drying;
wherein, the ultrasonic power of ultrasonic treatment is 1000W, and the frequency is 50kHz;
③ . Phosphating: preparing phosphating solution, wherein the phosphating solution comprises the following raw materials in parts by weight: 40 parts of phosphoric acid, 15 parts of nitric acid, 15 parts of zinc nitrate, 10 parts of citric acid, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of octyl phenol polyoxyethylene ether and 15 parts of water are sequentially placed into a stirrer, and uniformly stirred to obtain phosphating solution;
soaking the stainless steel plate in phosphating solution, carrying out ultrasonic oscillation treatment for 1-2 hours, taking out the stainless steel plate, washing with deionized water, and drying;
Step three: mixing of gases: the method comprises the steps that a seepage promoting agent dripping device is arranged above a heating container, nitrogen is introduced into the heating container, the seepage promoting agent is dripped into the heating container through the seepage promoting agent dripping device, the temperature in the heating container is increased, so that the gaseous seepage promoting agent is mixed with the nitrogen, and the mixing ratio of the gaseous seepage promoting agent to the nitrogen is 1:4, a step of;
Step four: ion nitriding: putting stainless steel into a vacuum ion nitriding furnace, adjusting the vacuum degree of the vacuum ion nitriding furnace to 35Pa, introducing helium gas to perform ion bombardment for 25min at the temperature of 330 ℃, stopping ion bombardment, and introducing mixed gas of a gaseous permeation accelerator and nitrogen, wherein the mixing ratio of the mixed gas of ammonia and hydrogen is 1:1.5, heating the temperature in the nitriding furnace to 530 ℃, regulating the pressure in the vacuum nitriding furnace to 140Mpa, maintaining the treatment time for 5h, stopping introducing the mixed gas of the gaseous catalyst and nitrogen, introducing the mixed gas of ammonia and hydrogen into the vacuum ion nitriding furnace, increasing the pressure in the furnace to 170Mpa, and continuing for 1.5h to complete nitriding;
Step five: oxidation reaction: stopping introducing oxygen into the mixed gas of ammonia and hydrogen, continuing for 1.5h when the temperature in the vacuum nitriding furnace is reduced to 350 ℃, stopping introducing oxygen after an oxide film is formed on the surface of the stainless steel, introducing ammonia, and cooling to room temperature along with the furnace after the temperature is reduced to 220 ℃.
Examples
An ion nitriding composite surface modification treatment method comprises the following steps:
Step one: cutting stainless steel plates: selecting a stainless steel plate, cutting the stainless steel plate by using a laser cutting machine, and polishing the cut part of the stainless steel plate by using a mirror surface polisher;
Step two: stainless steel sheet surface treatment:
① . Deoiling: preparing a chemical degreasing agent, wherein the chemical degreasing agent comprises the following raw materials in parts by weight: 40 parts of sodium hydroxide, 15 parts of sodium phosphate, 15 parts of emulsifying agent, 5 parts of trisodium phosphate, 3 parts of triethanolamine and the balance of water, and sequentially placing 40 parts of sodium hydroxide, 15 parts of sodium phosphate, 15 parts of emulsifying agent, 5 parts of trisodium phosphate, 3 parts of triethanolamine and 22 parts of water into a stirrer, and uniformly stirring to obtain a chemical degreasing agent;
Soaking the stainless steel plate in a chemical degreasing agent for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
② . Acid-base composite treatment: soaking the deoiled stainless steel plate in a sodium hydroxide solution with the mass concentration of 1-3% for 30min, performing ultrasonic treatment for 5min, taking out, cleaning with deionized water, and drying; then soaking the stainless steel plate in sulfuric acid with the mass concentration of 3% for 30min, carrying out ultrasonic treatment for 5min, taking out, cleaning with deionized water, and drying;
wherein, the ultrasonic power of ultrasonic treatment is 1000W, and the frequency is 50kHz;
③ . Phosphating: preparing phosphating solution, wherein the phosphating solution comprises the following raw materials in parts by weight: 40 parts of phosphoric acid, 15 parts of nitric acid, 15 parts of zinc nitrate, 10 parts of citric acid, 3 parts of sodium dodecyl benzene sulfonate, 2 parts of octyl phenol polyoxyethylene ether and 15 parts of water are sequentially placed into a stirrer, and uniformly stirred to obtain phosphating solution;
soaking the stainless steel plate in phosphating solution, carrying out ultrasonic oscillation treatment for 1-2 hours, taking out the stainless steel plate, washing with deionized water, and drying;
Step three: mixing of gases: the method comprises the steps that a seepage promoting agent dripping device is arranged above a heating container, nitrogen is introduced into the heating container, the seepage promoting agent is dripped into the heating container through the seepage promoting agent dripping device, the temperature in the heating container is increased, so that the gaseous seepage promoting agent is mixed with the nitrogen, and the mixing ratio of the gaseous seepage promoting agent to the nitrogen is 1:4, a step of;
step four: ion nitriding: putting stainless steel into a vacuum ion nitriding furnace, adjusting the vacuum degree of the vacuum ion nitriding furnace to be 30Pa, introducing helium gas to perform ion bombardment for 20min at the temperature of 350 ℃, stopping ion bombardment, and introducing mixed gas of a gaseous permeation accelerator and nitrogen, wherein the mixing ratio of the mixed gas of ammonia and hydrogen is 1:1.5, heating the temperature in the nitriding furnace to 550 ℃, regulating the pressure in the vacuum nitriding furnace to 150Mpa, maintaining the treatment time for 4h, stopping introducing the mixed gas of the gaseous catalyst and nitrogen, introducing the mixed gas of ammonia and hydrogen into the vacuum ion nitriding furnace, increasing the pressure in the furnace to 200Mpa, and continuing for 1h to finish nitriding;
Step five: oxidation reaction: stopping introducing oxygen into the mixed gas of ammonia and hydrogen, continuously cooling for 1h when the temperature in the vacuum nitriding furnace is reduced to 400 ℃, stopping introducing oxygen after an oxide film is formed on the surface of the stainless steel, introducing ammonia, and cooling to room temperature along with the furnace after the temperature is reduced to 250 ℃.
By using the technical scheme of the invention or under the inspired by the technical scheme of the invention, a similar technical scheme is designed by a person skilled in the art, so that the technical effects are achieved, and the technical effects fall into the protection scope of the invention.

Claims (6)

1. An ion nitriding composite surface modification treatment method is characterized in that: the method comprises the following steps:
Step one: cutting stainless steel plates: selecting a stainless steel plate, cutting the stainless steel plate by using a laser cutting machine, and polishing the cut part of the stainless steel plate by using a mirror surface polisher;
Step two: stainless steel sheet surface treatment:
① . Deoiling: soaking the stainless steel plate in a chemical degreasing agent for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
② . Acid-base composite treatment: soaking the deoiled stainless steel plate in a sodium hydroxide solution with the mass concentration of 1-3% for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying; soaking the stainless steel plate in 1-3% sulfuric acid for 20-30min, performing ultrasonic treatment for 3-5min, taking out, cleaning with deionized water, and drying;
③ . Phosphating: soaking the stainless steel plate in phosphating solution, carrying out ultrasonic oscillation treatment for 1-2 hours, taking out the stainless steel plate, washing with deionized water, and drying;
Step three: mixing of gases: a seepage catalyst dripping device is arranged above the heating container, nitrogen is introduced into the heating container, the seepage catalyst is dripped into the heating container through the seepage catalyst dripping device, and the temperature in the heating container is increased, so that the gaseous seepage catalyst is mixed with the nitrogen;
Step four: ion nitriding: placing stainless steel into a vacuum ion nitriding furnace, regulating the vacuum degree of the vacuum ion nitriding furnace to be 30-40Pa, introducing helium gas to perform ion bombardment for 20-30min at the temperature of 300-350 ℃, stopping ion bombardment, introducing mixed gas of a gaseous catalyst and nitrogen, heating the temperature in the nitriding furnace to 500-550 ℃, regulating the pressure in the vacuum nitriding furnace to be 130-150Mpa, maintaining the treatment time for 4-6h, stopping introducing the mixed gas of the gaseous catalyst and nitrogen, introducing mixed gas of ammonia and hydrogen into the vacuum ion nitriding furnace, increasing the pressure in the furnace to 150-200Mpa, and continuing for 1-2h, so that nitriding is completed;
Step five: oxidation reaction: stopping introducing oxygen into the mixed gas of ammonia and hydrogen, continuously cooling to room temperature along with the furnace after the temperature in the vacuum nitriding furnace is reduced to 300-400 ℃ for 1-2h and stopping introducing oxygen after an oxide film is formed on the surface of stainless steel, and introducing ammonia after the temperature is reduced to 200-250 ℃.
2. The ion nitriding composite surface modification treatment method according to claim 1, characterized by comprising the following steps: the chemical degreasing agent in the second step comprises the following raw materials in parts by weight: 40-50 parts of sodium hydroxide, 10-20 parts of sodium phosphate, 10-20 parts of emulsifying agent, 1-5 parts of trisodium phosphate, 1-3 parts of triethanolamine and the balance of water.
3. The ion nitriding composite surface modification treatment method according to claim 1, characterized by comprising the following steps: and in the second step, the ultrasonic power of ultrasonic treatment is 1000W, and the frequency is 50kHz.
4. The ion nitriding composite surface modification treatment method according to claim 1, characterized by comprising the following steps: the phosphating solution in the second step comprises the following raw materials in parts by weight: 20-40 parts of phosphoric acid, 10-20 parts of nitric acid, 10-20 parts of zinc nitrate, 5-10 parts of citric acid, 1-3 parts of sodium dodecyl benzene sulfonate, 1-2 parts of octyl phenol polyoxyethylene ether and the balance of water.
5. The ion nitriding composite surface modification treatment method according to claim 1, characterized by comprising the following steps: in the third step, the mixing ratio of the gaseous catalyst to the nitrogen is 1:4.
6. The ion nitriding composite surface modification treatment method according to claim 1, characterized by comprising the following steps: in the fourth step, the mixing ratio of the mixed gas of ammonia and hydrogen is 1:1.5.
CN202410402784.4A 2024-04-03 2024-04-03 Ion nitriding composite surface modification treatment method Pending CN118048601A (en)

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