CN112226724B - Normal-temperature nitriding process and processing device based on laser thermal-mechanical effect - Google Patents

Normal-temperature nitriding process and processing device based on laser thermal-mechanical effect Download PDF

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CN112226724B
CN112226724B CN202010950538.4A CN202010950538A CN112226724B CN 112226724 B CN112226724 B CN 112226724B CN 202010950538 A CN202010950538 A CN 202010950538A CN 112226724 B CN112226724 B CN 112226724B
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laser
laser beam
workpiece
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nitriding process
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CN112226724A (en
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汪卉
孟宪凯
周建忠
黄舒
李礼
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Jiangsu University
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Jiangsu University
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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
    • C23C8/08Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases only one element being applied
    • C23C8/24Nitriding
    • 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

Abstract

The invention provides a normal temperature state nitriding process and a processing device based on laser thermal-mechanical effect, comprising the following steps: filling ammonia gas into a closed box body in which a workpiece to be nitrided is placed at normal temperature; outputting a first laser beam and a second laser beam having different energies by a diffraction beam splitter; a plurality of second laser beams are focused above the surface of the workpiece, and the ammonia gas is ionized to form free nitrogen atoms through the laser thermal effect; the plurality of second laser beams are distributed around the first laser beam, the first laser beam irradiates the surface of the workpiece, and plasma generated by laser carries nitrogen atoms to penetrate into the surface of the workpiece along motion dislocation induced by force effect. The invention uses the thermal effect and the force effect of the laser to carry out surface strengthening treatment, can obtain higher strength, hardness and fatigue performance than single strengthening treatment, and can improve the defect of coarse grains caused by conventional high-temperature nitriding by normal-temperature nitriding.

Description

Normal-temperature nitriding process and processing device based on laser thermal-mechanical effect
Technical Field
The invention relates to the technical field of heat treatment or surface nitriding, in particular to a normal-temperature nitriding process and a processing device based on a laser thermal-force effect.
Background
Nitriding, i.e. a chemical heat treatment process for making nitrogen atoms penetrate into the surface layer of a workpiece in a certain medium at a certain temperature. In the traditional gas nitriding process, a workpiece is placed in a sealed container, flowing ammonia gas is introduced and heated, after the heat preservation is carried out for a long time, the ammonia gas is thermally decomposed to generate active nitrogen atoms, the active nitrogen atoms are continuously adsorbed to the surface of the workpiece and are diffused and permeated into the surface layer of the workpiece, so that the chemical components and the structure of the surface layer are changed, and the excellent surface performance is obtained. The invention discloses a nitriding treatment process of a high-speed steel cutter, namely a layer of compact oxidation film, namely a nitriding layer, is formed on the surface of the high-speed steel cutter through nitriding treatment. But the traditional nitriding has the defect of long high-temperature treatment time.
In order to improve the nitriding effect and increase the thickness of the nitriding layer, a plurality of pretreatments can be carried out to achieve the purpose. The invention discloses a laser shock process for improving ion nitriding efficiency, namely, a workpiece is subjected to laser shock treatment and then placed in an ion nitriding furnace for ion nitriding treatment. The Chinese patent of the invention discloses a laser high-temperature impact-nitriding composite processing device and a method, namely, laser impact strengthening and nitriding treatment are respectively carried out, high-density dislocation, dislocation entanglement and subboundary are generated on the surface of a material, and nitrogen atoms and metal atoms are induced to generate high-temperature phase change reaction. The above two patents utilize laser shock pretreatment to increase the dislocation density on the surface of the material, and then carry out nitriding treatment to induce nitrogen atoms to penetrate into the material along the dislocations, but the method also has certain defects: firstly, the traditional nitriding treatment time is too long, and the traditional nitriding high temperature causes large grains, so that the phenomenon of grain refining caused by laser shock strengthening is weakened, and the whole strengthening effect is influenced.
Disclosure of Invention
Aiming at the defects of long time and large grains induced by high temperature in the prior art in the traditional nitriding treatment, the invention provides a normal temperature state nitriding process and a processing device based on a laser thermal-force effect, ammonia gas is ionized through the laser thermal effect, more nitrogen atoms are adsorbed on the surface of a sample, moving dislocation is taken as a nitriding channel, the thickness of a nitriding layer can be increased, and the defect of large grains of the traditional high temperature nitriding induced material is avoided; high-density dislocation is generated on the surface of the material through the induction of the laser force effect, and plasma generated by laser shock peening is used as a carrier, so that nitrogen atoms can be carried along a grain boundary and the moving dislocation to permeate into the material, and the strength, hardness and fatigue performance of a nitriding layer can be further improved.
The present invention achieves the above-described object by the following technical means.
A normal temperature state nitriding process based on laser thermal-mechanical effect comprises the following steps:
filling ammonia gas into a closed box body in which a workpiece to be nitrided is placed at normal temperature;
outputting a first laser beam and a second laser beam having different energies by a diffraction beam splitter; a plurality of second laser beams are focused above the surface of the workpiece, and the ammonia gas is ionized to form free nitrogen atoms through the laser thermal effect; the plurality of second laser beams are distributed around the first laser beam, the first laser beam irradiates the surface of the workpiece, and plasma generated by laser carries nitrogen atoms to penetrate into the surface of the workpiece along motion dislocation induced by force effect.
Further, the energy of the first laser beam is smaller than the energy of the second laser beam.
Further, the ratio of the energy of the first laser beam to the energy of the second laser beam is 4: 6.
Further, the diameter of a light spot focused by the first laser beam is not less than 3mm, and the diameter of a light spot focused by the second laser beam is 0.2-0.8 mm.
Further, a plurality of second laser beams are focused 0.2-0.5 mm above the surface of the workpiece.
A processing device of normal temperature nitriding process based on laser heat-force effect comprises a laser, a seal box, a diffraction beam splitter and an ammonia device; a workpiece to be nitrided is placed in the seal box, the laser is used for emitting laser, the diffraction beam splitter is used for splitting the laser emitted by the laser into a first laser beam and a second laser beam with different energy, and the second laser beams are distributed around the first laser beam; a plurality of second laser beams are focused above the surface of the workpiece through the sealing box, and the first laser beams are focused on the surface of the workpiece through the sealing box; the seal box is communicated with an ammonia device.
Further, the device also comprises a combined lens A, a combined lens B, a reflecting mirror and a focusing mirror; the first laser beam and the second laser beam sequentially pass through a combined lens A, a reflector and a combined lens B and then enter a sealing box, the combined lens A is used for collimating the first laser beam and the second laser beam, and the combined lens B is used for deflecting the first laser beam and the second laser beam; and a focusing mirror is arranged in the sealed box and used for focusing the deflected first laser beam and the deflected second laser beam to a workpiece to be nitrided.
The invention has the beneficial effects that:
1. according to the normal-temperature nitriding process based on the laser thermal-force effect, ammonia gas is ionized through the laser thermal effect, more nitrogen atoms are adsorbed on the surface of a sample, moving dislocation is used as a nitriding channel, the thickness of a nitriding layer can be increased, and the defect that grains of a traditional high-temperature nitriding induction material are thick is avoided; high-density dislocation is generated on the surface of the material through the induction of the laser force effect, and plasma generated by laser shock peening is used as a carrier, so that nitrogen atoms can be carried along a grain boundary and the moving dislocation to permeate into the material, and the strength, hardness and fatigue performance of a nitriding layer can be further improved.
2. The normal-temperature nitriding process based on the laser thermal-force effect utilizes the thermal effect and the force effect of the laser to carry out surface strengthening treatment, and can obtain higher strength, hardness and fatigue performance than single strengthening treatment.
3. The normal temperature state nitriding process based on the laser thermal-mechanical effect takes the moving dislocation as a nitriding channel, can increase the thickness of a nitriding layer and improve the nitriding uniformity, and avoids the normal temperature state nitriding treatment at the same time.
4. According to the normal-temperature nitriding process based on the laser thermal-mechanical effect, the surface dislocation motion is increased by using the mechanical effect of the laser, the defects such as sub-grain boundary and dislocation are formed, and the surface has high-amplitude residual compressive stress, so that nitrogen atoms are promoted to diffuse into a matrix along the moving dislocation, and the strength, hardness and fatigue performance of a nitriding layer are further improved.
5. The normal-temperature nitriding process based on the laser thermal-force effect provided by the invention has the advantages that the ionization is generated above the surface of the workpiece by using the thermal effect of the laser, so that a large number of nitrogen atoms are attached to the surface of the workpiece, and the plasma generated by the force effect of the laser is used as a carrier and can carry a part of the nitrogen atoms to permeate into the material.
6. The processing device of the normal temperature state nitriding process based on the laser thermal-force effect reduces the material clamping time in the composite processing process, improves the working efficiency and is simpler and more convenient to operate. In addition, the device provided by the invention performs nitriding at normal temperature, and compared with the traditional nitriding process which needs high-temperature treatment, the device provided by the invention shortens the processing time to a great extent.
Drawings
FIG. 1 is a schematic view of a processing device of a normal temperature state nitriding process based on a laser thermal-mechanical effect.
In the figure:
1-a laser; a 2-diffraction beam splitter; 3-a combined lens a; 4-a pressure sensor; 5-air inlet flow valve; 6-a reflector; 7-a combined lens B; 8-high temperature and high pressure resistant quartz glass; 9-sealing the box; 10-outlet flow valve; 11-waste gas storage bottle; 12-a first focusing mirror; 13-a three-axis linkage workbench; 14-a workpiece; 15-a second focusing mirror; 16-ammonia cylinders; 17-computer.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, but the scope of the invention is not limited thereto.
As shown in fig. 1, the processing device of the normal temperature state nitriding process based on the laser thermal-mechanical effect comprises a laser 1, a seal box 9, a diffraction beam splitter 2, a combined lens a3, a combined lens B7, a reflector 6, a first focusing mirror 12, a second focusing mirror 15 and an ammonia bottle 16; a workpiece 14 to be nitrided is placed in the seal box 9, and a three-axis linkage workbench 13 is arranged at the bottom of the workpiece 14 to be nitrided and used for three-dimensional movement of the workpiece 14 to be nitrided. The upper part of the sealing box 9 is provided with high temperature and high pressure resistant quartz glass 8, laser irradiates on a workpiece 14 through the high temperature and high pressure resistant quartz glass 8, and the ammonia gas bottle 16 and the waste gas storage bottle 11 are respectively connected with the sealing box 9 through gas pipes. An air inlet flow valve 5 is arranged between the ammonia bottle 16 and the sealing box 9, and an air outlet flow valve 10 is arranged between the waste gas storage bottle 11 and the sealing box 9. When the ammonia gas works, the air pressure is maintained at 150-300Pa, and the computer 17 adjusts the flow inlet and outlet valves according to the information fed back by the pressure sensor 4 to realize the closed-loop control of the pressure in the sealing box.
The laser 1 is used for emitting laser, and the laser 1 is a nanosecond pulse laser with a laser pulse width of 20-25 ns. The diffraction beam splitter 2 is used for splitting laser emitted by the laser 1 into a first laser beam and a second laser beam with different energies, and a plurality of the second laser beams are distributed around the first laser beam; a number of said second laser beams are focused above the workpiece surface through the sealing box 9, said first laser beams are focused on the workpiece surface through the sealing box 9; the seal box 9 is communicated with an ammonia device. The first laser beam and the second laser beam sequentially pass through a combined lens A3, a reflecting mirror 6 and a combined lens B7 and then enter a sealed box 9, the combined lens A3 is used for collimating the first laser beam and the second laser beam, and the combined lens B7 is used for deflecting the first laser beam and the second laser beam; a first focusing mirror 12 and a second focusing mirror 15 are installed in the sealed box 9 and used for enabling the deflected first laser beam and the deflected second laser beam to be focused on a workpiece to be nitrided.
The surface strengthening treatment is carried out by using the normal temperature nitriding process based on the laser thermal-mechanical effect of the invention by taking Cr12MoV cold-work die steel with the size of 30mm multiplied by 5mm as an example. The method comprises the following specific steps:
and (3) polishing the workpiece 14 to be nitrided to a mirror surface by using #400 to #2000 SiC abrasive paper, performing ultrasonic cleaning by using absolute ethyl alcohol, and placing the workpiece on the three-axis linkage workbench 13.
And opening the pressure sensor 4, introducing ammonia gas, and regulating an inflow and outflow valve by a computer according to information fed back by the pressure sensor 4 to realize closed-loop control of the pressure in the sealing box and control the pressure in the sealing box to be maintained at about 200 Pa.
After the pressure in the sealed box is stable, the parameters of the laser 1 are set to be 25ns of pulse width and 30J of laser energy.
Opening the diffraction beam splitter 2, splitting laser emitted by the laser 1 into a first laser beam and a second laser beam with different energies, focusing a plurality of second laser beams above the surface of the workpiece 14 to be nitrided, and ionizing ammonia gas to form free nitrogen atoms through the laser thermal effect; a plurality of second laser beams are distributed around the first laser beam, the first laser beam irradiates a workpiece 14 to be nitrided, and plasma generated by laser carries nitrogen atoms to permeate into the surface of the workpiece along motion dislocation induced by force effect; the energy of the first laser beam was 12J and the energy of the second laser beam was 18J.
The spot diameter of each laser beam is adjusted through the focusing lens, the size of a spot corresponding to the first laser beam is 3mm, the size of a spot corresponding to the second laser beam is 0.6mm, and the height of the focus of the second laser beam from the surface of the workpiece is 0.3 mm.
The three-axis workbench 13 moves according to a preset path until the processing is finished, and the overlapping rate of the laser beam spots corresponding to the force effect is ensured to be 50% in the process.
After the processing is finished, waste gas is collected to the seal box, the waste gas is collected in a waste gas storage bottle, and then the workpiece is unloaded.
The laser, the diffracted beam splitter, and the pressure sensor are turned off.
The thickness of the processed nitriding layer of the Cr12MoV workpiece can be expected to reach 60-70 mu m, and a connecting line between the nitriding layer and the base material can be relatively flat.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.

Claims (7)

1. A normal temperature state nitriding process based on laser thermal-mechanical effect is characterized by comprising the following steps:
filling ammonia gas into a closed box body in which a workpiece to be nitrided is placed at normal temperature;
outputting a first laser beam and a second laser beam having different energies by a diffraction beam splitter (2); a plurality of second laser beams are focused above the surface of the workpiece, and the ammonia gas is ionized to form free nitrogen atoms through the laser thermal effect; the plurality of second laser beams are distributed around the first laser beam, the first laser beam irradiates the surface of the workpiece, and plasma generated by laser carries nitrogen atoms to penetrate into the surface of the workpiece along motion dislocation induced by force effect.
2. The normal-temperature nitriding process based on laser thermo-mechanical effect according to claim 1, wherein the energy of the first laser beam is smaller than the energy of the second laser beam.
3. The normal-temperature nitriding process based on laser thermo-mechanical effect according to claim 1, wherein the ratio of the energy of the first laser beam to the energy of the second laser beam is 4: 6.
4. The normal-temperature nitriding process based on the laser thermal-mechanical effect as claimed in claim 1, wherein the diameter of a focused spot of the first laser beam is not less than 3mm, and the diameter of a focused spot of the second laser beam is 0.2-0.8 mm.
5. The normal-temperature nitriding process based on the laser thermo-mechanical effect as claimed in claim 1, wherein a plurality of the second laser beams are focused 0.2-0.5 mm above the surface of the workpiece.
6. A processing device of normal temperature nitriding process based on laser thermo-mechanical effect according to claim 1, characterized by comprising a laser (1), a sealed box (9), a diffraction beam splitter (2) and an ammonia gas device; a workpiece to be nitrided is placed in the seal box (9), the laser (1) is used for emitting laser, the diffraction beam splitter (2) is used for splitting the laser emitted by the laser (1) into a first laser beam and a second laser beam with different energy, and a plurality of second laser beams are distributed around the first laser beam; a number of said second laser beams are focused above the surface of the workpiece through the sealing box (9), said first laser beams are focused on the surface of the workpiece through the sealing box (9); the sealing box (9) is communicated with an ammonia device.
7. The processing device of normal temperature state nitriding process based on laser thermo-mechanical effect according to claim 6, characterized by further comprising a combination lens A (3), a combination lens B (7), a reflector (6) and a focusing mirror (12, 15); the first laser beam and the second laser beam sequentially pass through a combined lens A (3), a reflecting mirror (6) and a combined lens B (7) and then enter a sealing box (9), the combined lens A (3) is used for collimating the first laser beam and the second laser beam, and the combined lens B (7) is used for deflecting the first laser beam and the second laser beam; focusing mirrors (12, 15) are arranged in the sealing box (9) and are used for focusing the deflected first laser beam and the second laser beam to a workpiece to be nitrided.
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CN202010950538.4A CN112226724B (en) 2020-09-11 2020-09-11 Normal-temperature nitriding process and processing device based on laser thermal-mechanical effect
PCT/CN2020/133238 WO2022052334A1 (en) 2020-09-11 2020-12-02 Room-temperature nitriding process based on thermal-mechanical effects of laser, and processing device
GB2304209.6A GB2614984B (en) 2020-09-11 2020-12-02 Room-temperature nitriding process based on thermal-mechanical effects of laser, and processing device

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CN113026000B (en) * 2021-04-02 2022-12-09 泰杋科技股份有限公司 Device and method for preparing tantalum nitride film by precursor coating gas protection laser
CN115404436B (en) * 2022-05-07 2024-04-09 江苏大学 Ultrasonic acceleration-based surface strengthening device and method

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GB2614984B (en) 2024-02-14

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