CN111962058A - Method and device for implanting nano diamond particles on surface of alloy steel at high temperature - Google Patents
Method and device for implanting nano diamond particles on surface of alloy steel at high temperature Download PDFInfo
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- CN111962058A CN111962058A CN202010697128.3A CN202010697128A CN111962058A CN 111962058 A CN111962058 A CN 111962058A CN 202010697128 A CN202010697128 A CN 202010697128A CN 111962058 A CN111962058 A CN 111962058A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
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- C21D10/005—Modifying the physical properties by methods other than heat treatment or deformation by laser shock processing
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Abstract
The invention provides a method for implanting nano diamond particles on the surface of alloy steel at high temperature, which comprises the following steps: mixing nano diamond particles and industrial vaseline ointment in proportion, pre-coating the mixture on the surface of an alloy steel target to form a nano diamond coating, and then closely laying an absorption layer on the nano diamond coating; heating the alloy steel target material to a set temperature and then preserving heat; arranging a restraint layer on the absorption layer, and impacting the surface of the alloy steel target material by using high-energy short pulse laser according to a set lap joint rate; and after laser shock, removing the restraint layer, the absorption layer and the nano-diamond coating to obtain the nano-diamond superhard strengthening layer. The invention can improve the properties of alloy steel such as surface hardness, wear resistance, contact fatigue strength and the like.
Description
Technical Field
The invention relates to the technical field of metal surface modification, in particular to a method and a device for implanting nano diamond particles on the surface of alloy steel at a high temperature.
Background
The marine transmission gear has large size and complex stress, is generally made of 20Cr2Ni4A or 18Cr2Ni4WA alloy steel and the like, and has high alloy content and good hardenability. Because the requirement of the marine transmission gear on the hardness of the tooth surface is high, the strength and the wear resistance of the gear are improved mainly by heat treatment processes such as carburizing, nitriding, nitrocarburizing process, direct quenching or induction quenching and the like at present. However, after the gear is subjected to carburization treatment, the carburized layer has poor bonding performance and is easy to strip during heavy-load impact; in addition, too high carburizing temperature further aggravates the deformation of the gear, causes gear grains to be coarse, and reduces the mechanical property. The hardened layer formed by the nitriding technology is thin and is not suitable for the high-speed impact environment. In addition, if the requirement on the precision of the gear is high, the gear surface needs to be subjected to gear grinding after heat treatment so as to overcome the deformation of the heat treatment, and tensile stress can occur in the process of gear grinding, so that microcracks are initiated and expanded, and the fatigue life and the shock resistance of the gear are reduced.
Therefore, the development of a brand new method for alloy steel not only can avoid high-temperature deformation, but also can form a superhard strengthening layer on the surface has important significance and wide application prospect.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method and a device for implanting nano-diamond particles on the surface of alloy steel at high temperature, wherein the nano-diamond particles are implanted on the surface layer of the alloy steel to form a superhard strengthening layer by utilizing laser shock so as to improve the performances of the alloy steel, such as surface hardness, wear resistance, contact fatigue strength and the like.
The present invention achieves the above-described object by the following technical means.
A method for implanting nano-diamond particles on the surface of alloy steel at high temperature comprises the following steps:
mixing nano diamond particles and industrial vaseline ointment in proportion, pre-coating the mixture on the surface of an alloy steel target to form a nano diamond coating, and then closely laying an absorption layer on the nano diamond coating;
heating the alloy steel target material to a set temperature and then preserving heat;
arranging a restraint layer on the absorption layer, and impacting the surface of the alloy steel target material by using high-energy short pulse laser according to a set lap joint rate;
and after laser shock, removing the restraint layer, the absorption layer and the nano-diamond coating to obtain the nano-diamond superhard strengthening layer.
Further, before the nano diamond coating is pre-coated, the alloy steel target material is pretreated, and the pretreatment method comprises the following steps: cutting and sampling the annealed alloy steel, polishing the surface of the alloy steel step by using 400-1500-mesh metallographic water-milled sand paper, polishing the alloy steel to a mirror surface effect step by using a metallographic polishing agent with the specification of 0.5-3.5 mu m, finally ultrasonically cleaning the alloy steel target material in an absolute ethyl alcohol or acetone solution, and immediately drying the surface of the alloy steel target material after cleaning.
Further, the ratio of the nano diamond particles to the industrial vaseline ointment is 1: 1-5.
Further, the thickness range of the nano diamond particle coating is 0.05-1 mm.
Further, the size of the nano diamond particles is 1-250 nm.
Furthermore, the pulse width of the high-energy short pulse laser is 1-100 ns, the repetition frequency is 1-20Hz, and the laser power density is 1-100 GW/cm2The diameter of the laser spot is 1-10 mm, and the overlapping rate of the laser spot ranges from 50-70%.
Further, the absorbing layer is a black adhesive tape or black paint or an aluminum foil, and the thickness range of the absorbing layer is 0.1-1 mm.
Furthermore, the restraint layer is made of ionized water or K9 glass, and the thickness range of the restraint layer is 0.1-2 mm.
Further, the set temperature is not less than 450 ℃.
The device for realizing the method for implanting the nano-diamond particles on the surface of the alloy steel at the high temperature is characterized by comprising the following steps:
the laser shock processing equipment is used for carrying out laser shock processing; and
the heating equipment is used for heating the alloy steel target;
the heating equipment comprises a heating wire, a variable resistor, a contactor, a numerical control switch and a power supply, wherein the heating wire is coated on the alloy steel target material, and the heating wire, the variable resistor, the contactor, the numerical control switch and the power supply are sequentially connected in series to form a closed loop.
The invention has the beneficial effects that:
the alloy steel target is firstly heated to more than 450 ℃ by electrifying, so that the strength of the alloy steel target is greatly reduced, then the high-energy plasma explosion wave generated by impacting the alloy steel target by high-energy short pulse laser is utilized to bombard the high-strength pre-coated nano diamond coating preset on the surface of the alloy steel target at high speed, so that the nano diamond particles are implanted into the alloy steel surface layer to form a superhard strengthening layer, and meanwhile, the characteristics of low temperature, high pressure, ultrafast speed and the like in the laser impact process are utilized, so that the phenomena of graphitization and agglomeration of the implanted nano diamond particles are avoided, the self characteristics of the nano diamond particles are retained, the laser impact and nano diamond particle composite strengthening effect is achieved, and the performances of the surface hardness, the wear resistance, the contact fatigue.
Drawings
Fig. 1 is a schematic diagram of a method and an apparatus for implanting nano-diamond particles on the surface of alloy steel at a high temperature according to an embodiment of the present invention.
FIG. 2 is a schematic representation of the 50% overlap ratio and impact zone area of an example of the invention;
FIG. 3 is a partially enlarged schematic view of the nano-diamond particles implanted into the alloy steel surface layer after laser shock according to an embodiment of the invention;
FIG. 4 is a microstructure diagram of a 5nm diamond particle implanted alloy steel surface layer after laser shock according to an embodiment of the invention;
FIG. 5 is a microstructure of a surface layer of alloy steel implanted with 250nm diamond particles after laser shock according to an embodiment of the present invention;
FIG. 6 is a graph of the results of the hardness of the alloy steel section after laser shock according to an embodiment of the present invention;
FIG. 7 is a graph of the results of laser shock followed by tribological wear in accordance with embodiments of the present invention.
Reference numerals:
1. a controller; 2. a laser generator; 3. a high energy short pulse laser beam; 4. plasma; 5. a constraining layer; 6. an absorbing layer; 7. a nanodiamond coating; 8. alloy steel target material; 9. an electric heating wire; 10. a variable resistor; 11. a contactor; 12. a numerical control switch; 13. a power source.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but rather should be construed as broadly as the present invention is capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature comprises the following steps:
the method comprises the following steps: firstly, cutting and sampling the annealed alloy steel, gradually polishing the surface by using 400-1500-mesh metallographic abrasive paper, then gradually polishing the surface to a mirror surface effect by using a 0.5-3.5-micron metallographic polishing agent, finally ultrasonically cleaning the sample in an absolute ethyl alcohol or acetone solution, and immediately drying the surface after cleaning.
Step two: mixing and stirring the nano-diamond particles and the industrial vaseline ointment uniformly according to a proportion, then pre-coating the mixture on the surface of the alloy steel target material, then tightly laying a black adhesive tape, black paint or aluminum foil as an absorption layer on the nano-diamond coating, and drying for 24 hours at room temperature.
Step three: the alloy steel target is electrified and heated to more than 450 ℃ by a heating device and then is insulated.
Step four: deionized water or K9 glass is selected as a restraint layer and is arranged on the absorption layer, and high-energy short pulse laser is used for impacting and sequentially covering the restraint layer, the absorption layer and the alloy steel target surface pre-coated with the nano diamond coating according to a selected lap joint rate.
Step five: after laser impact, firstly removing the heating device, after the air cooling of the alloy steel target to room temperature, sequentially removing the restraint layer, the absorption layer and the pre-laid nano-diamond coating, then ultrasonically cleaning the sample in absolute ethyl alcohol or acetone solution, immediately drying the surface after cleaning, and implanting nano-diamond particles to the surface of the alloy steel to obtain the nano-diamond superhard strengthening layer.
Further, in the method of the embodiment of the invention, the size of the nano-diamond particles is 1-250 nm, and the thickness of the nano-diamond particle layer is 0.05-1 mm.
Further, in the method of the embodiment of the present invention, the mixing ratio of the nano diamond powder and the industrial vaseline ointment is in the range of 1: 1-5, the thickness range of the absorption layer is 0.1-1 mm, and the thickness range of the restraint layer is 0.1-2 mm.
Furthermore, in the method of the embodiment of the invention, the range of the high-energy short pulse laser impact parameter is 1-100 ns in pulse width, and the laser power density is 1-100 GW/cm2The diameter of the laser spot is 1-10 mm, and the overlapping rate of the laser spot ranges from 50% to 70%.
The invention firstly heats the alloy steel target material to more than 450 ℃ by electrifying, at the moment, the carbide in the pearlite of the alloy steel structure obtains energy to be transferred and gathered, and is converted from a sheet shape to a spherical shape, so that the sheet-shaped graphitization phenomenon with extremely low strength is precipitated to promote the embrittlement of the alloy steel, the strength and the plasticity are greatly reduced, and the strength difference is generated between the alloy steel structure and the nano diamond particles, then the high-energy plasma explosion wave generated by impacting the alloy steel target material by high-energy short pulse laser is utilized to bombard the high-strength pre-coated nano diamond coating preset on the surface of the alloy steel target material at high speed, so that the nano diamond particles are implanted into the surface layer of the alloy steel to form the superhard strengthening layer, and meanwhile, the characteristics of low temperature, high pressure, ultrafast speed and the like in the laser impact process are utilized, the phenomena of graphitization and, and the surface hardness, the wear resistance, the contact fatigue strength and other properties of the material are also improved.
An apparatus for implementing the method for implanting the nano-diamond particles on the surface of the alloy steel at the high temperature comprises: the device comprises laser impact processing equipment and heating equipment, wherein the laser impact processing equipment is used for carrying out laser impact processing, and the heating equipment is used for heating the alloy steel target. The heating equipment comprises a heating wire, a variable resistor, a contactor, a numerical control switch and a power supply, the heating wire is coated on the alloy steel target material, the heating wire, the variable resistor, the contactor, the numerical control switch and the power supply are sequentially connected in series to form a closed loop, the alloy steel target material is heated by the heating wire coated on the alloy steel target material, and the heating is uniform and efficient.
Example 1
20Cr2Ni4A steel is a high-quality alloy carburizing steel, is mainly used for manufacturing gear parts of heavy-duty vehicles and ships, and is required to have high surface hardness and good contact fatigue strength industrially, so that strengthening treatment such as carburizing, nitriding, ultrasonic impact and the like is often required. In the carburizing process, the defects of grain growth, a large amount of unconverted residual austenite on the surface and the like can occur, thereby affecting the fatigue life and the reliability of the workpiece. The invention is implemented in the laser shock implantation of nano-diamond particles on the surface of 20Cr2Ni4A steel, and specifically comprises the following steps:
the method comprises the following steps: firstly, cutting an annealed 20Cr2Ni4A steel wire into samples with the size of 15 multiplied by 10mm, then gradually polishing the surfaces of the samples by using 400-1500-mesh metallographic abrasive paper, gradually polishing the surfaces of the samples to a mirror surface effect by using 0.5-3.5 mu m metallographic polishing agent, finally ultrasonically cleaning the samples in absolute ethyl alcohol or acetone solution, and immediately drying the surfaces of the samples after cleaning;
step two: mixing 5nm diamond particles and industrial vaseline ointment according to the weight ratio of 1: 5, mixing and stirring uniformly, then pre-coating the mixture on the surface of 20Cr2Ni4A steel to obtain a nano-diamond coating with the thickness of 0.2mm, selecting aluminum foil adhesive tape paper with the thickness of 0.12mm as an absorption layer to tightly cover the pre-coated nano-diamond coating, and drying the nano-diamond coating for 24 hours at room temperature.
Step three: and electrifying and heating the alloy steel target to 500 ℃ by a heating device, and then preserving heat.
Step four: deionized water (2mm) is selected as a restraint layer and is placed on the absorption layer, and the used laser impact parameter is 1064 nm; pulse width 10 ns; the effective light spot diameter is 3 mm; the repetition frequency is 5 Hz; laser power density 17GW/cm2Single pulse energy 12J. As shown in figure 2, the surface of the 20Cr2Ni4A steel target material which is sequentially covered with the restraint layer, the absorption layer and the pre-coated nano diamond coating is impacted according to the lap ratio of 50 percent, and the area of the impact area is 12 multiplied by 12mm2。
Step five: after laser impact, firstly removing the heating device, after the air cooling of the alloy steel target to room temperature, sequentially removing the restraint layer, the absorption layer and the pre-laid nano-diamond coating in sequence, then ultrasonically cleaning the sample in absolute ethyl alcohol or acetone solution, and immediately drying the surface after cleaning to obtain the nano-diamond superhard strengthening layer.
Example 2
The size of the diamond particles in step one of implementation 1 was changed to 250nm, and the remaining steps were unchanged.
After the treatment by the method and the device for implanting the nano-diamond particles on the surface of the 20Cr2Ni4A steel at high temperature through laser impact, the fact that the diamond particles of 5nm are implanted on the surface layer of the 20Cr2Ni4A steel is shown in fig. 4(b), the maximum Vickers hardness of the surface reaches 213HV, the depth of a hardened layer reaches 0.2mm compared with that of the original sample, and as shown in fig. 6, the implanted nano-diamond also reduces the friction coefficient of the target, as shown in fig. 7, the laser impact effect causes the surface roughness of the target to be improved, so that the friction coefficient of the sample fluctuates in 0 to 300s, but in 300 to 600s, the friction coefficient of the target with the nano-diamond is obviously lower than that of the original sample, better wear resistance is shown, the residual compressive stress is-207 MPa, the depth reaches 1.2mm, and the physical performance of the 20Cr2Ni4A steel is obviously improved; secondly, in fig. 4(a) and 5(b), some nano-diamond particles were also found to leave pits and stress cracks in the shape of ripples after being detached, which also indicates that the nano-diamond was successfully implanted on the surface of 20Cr2Ni4A steel rather than adhesion effect.
Similarly, 250nm diamond particles are also successfully implanted into the surface layer of 20Cr2Ni4A steel as shown in FIG. 5(b), the maximum Vickers hardness of the surface reaches 187HV, which is improved by 16.9% compared with the original sample, the depth of a hardened layer reaches 0.2mm, as shown in FIG. 6, the residual compressive stress reaches up to-177 MPa, and the depth reaches 0.8mm, thus verifying the feasibility of the method.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A method for implanting nano-diamond particles on the surface of alloy steel at high temperature is characterized by comprising the following steps:
mixing nano diamond particles and industrial vaseline ointment in proportion, pre-coating the mixture on the surface of an alloy steel target to form a nano diamond coating, and then closely laying an absorption layer on the nano diamond coating;
heating the alloy steel target material to a set temperature and then preserving heat;
arranging a restraint layer on the absorption layer, and impacting the surface of the alloy steel target material by using high-energy short pulse laser according to a set lap joint rate;
and after laser shock, removing the restraint layer, the absorption layer and the nano-diamond coating to obtain the nano-diamond superhard strengthening layer.
2. The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature according to claim 1, wherein the pretreatment is carried out on the alloy steel target material before the nano-diamond coating is pre-coated, and the pretreatment method comprises the following steps: cutting and sampling the annealed alloy steel, polishing the surface of the alloy steel step by using 400-1500-mesh metallographic water-milled sand paper, polishing the alloy steel to a mirror surface effect step by using a metallographic polishing agent with the specification of 0.5-3.5 mu m, finally ultrasonically cleaning the alloy steel target material in an absolute ethyl alcohol or acetone solution, and immediately drying the surface of the alloy steel target material after cleaning.
3. The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature according to claim 1, wherein the ratio of the nano-diamond particles to the industrial vaseline ointment is 1: 1-5.
4. The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature according to claim 1, wherein the thickness of the nano-diamond particle coating ranges from 0.05 mm to 1 mm.
5. The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature according to claim 1, wherein the size of the nano-diamond particles is 1-250 nm.
6. The method for implanting nano-diamond particles on the surface of alloy steel at high temperature according to claim 1, wherein the pulse width of the high-energy short pulse laser is 1-100 ns, the repetition frequency is 1-20Hz, and the laser power density is 1-100 GW/cm2The diameter of the laser spot is 1-10 mm, and the overlapping rate of the laser spot ranges from 50-70%.
7. The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature according to claim 1, wherein the absorption layer is black tape, black paint or aluminum foil, and the thickness of the absorption layer ranges from 0.1 mm to 1 mm.
8. The method for implanting the nano-diamond particles into the surface of the alloy steel at the high temperature according to claim 1, wherein the constraint layer is ionized water or K9 glass, and the thickness of the constraint layer ranges from 0.1 mm to 2 mm.
9. The method for implanting nanodiamond particles into the surface of alloy steel at high temperature according to claim 1, wherein the set temperature is not less than 450 ℃.
10. An apparatus for implementing the method for implanting nano-diamond particles on the surface of alloy steel at high temperature according to claim 1, which comprises:
the laser shock processing equipment is used for carrying out laser shock processing; and
the heating equipment is used for heating the alloy steel target;
the heating equipment comprises a heating wire, a variable resistor, a contactor, a numerical control switch and a power supply, wherein the heating wire is coated on the alloy steel target material, and the heating wire, the variable resistor, the contactor, the numerical control switch and the power supply are sequentially connected in series to form a closed loop.
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| CN112647083A (en) * | 2020-11-24 | 2021-04-13 | 江苏大学 | Alloy steel surface composite strengthening process |
| CN112958917A (en) * | 2021-02-05 | 2021-06-15 | 中国航发中传机械有限公司 | Laser impact marking method for metal components |
| CN113967796A (en) * | 2021-10-26 | 2022-01-25 | 江苏大学 | Method for preparing super-hydrophobic surface by laser shock imprinting of micro-nano particles on surface of aluminum alloy |
| CN115058584A (en) * | 2022-05-13 | 2022-09-16 | 西安交通大学 | Device and method for assisting laser temperature strengthening by metal particles |
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