CN111607760A - M50 steel pulse electron beam irradiation Nb-W-Cr-Mo alloying method - Google Patents
M50 steel pulse electron beam irradiation Nb-W-Cr-Mo alloying method Download PDFInfo
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- CN111607760A CN111607760A CN201911107661.3A CN201911107661A CN111607760A CN 111607760 A CN111607760 A CN 111607760A CN 201911107661 A CN201911107661 A CN 201911107661A CN 111607760 A CN111607760 A CN 111607760A
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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
- 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
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
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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
- 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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
- C23C14/28—Vacuum evaporation by wave energy or particle radiation
- C23C14/30—Vacuum evaporation by wave energy or particle radiation by electron bombardment
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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
- 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
- C23C14/22—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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
Abstract
The invention discloses an M50 steel pulse electron beam irradiation Nb-W-Cr-Mo alloying method, and belongs to the field of M50 steel surface treatment. The invention aims to solve the problem of low high-temperature frictional wear resistance of M50 steel. The method comprises the following steps: firstly, pretreating the surface of an M50 steel workpiece; secondly, placing the workpiece on a workbench in a vacuum chamber, facing the surface to be processed of the workpiece to an electron gun, and vacuumizing; thirdly, continuously introducing argon into the vacuum chamber, and irradiating; fourthly, performing magnetron sputtering on the surface to be treated of the workpiece by using a Mo target material, a Cr target material, a W target material and a Nb target material in sequence; fifthly, turning the surface to be processed of the workpiece to face the electron beam, introducing argon into the vacuum chamber, and irradiating for 50-100 times; sixthly, taking out the product after cooling and cooling the product in air to finish the process. The method reduces the high-temperature friction coefficient of the M50 steel and improves the high-temperature friction and wear resistance.
Description
Technical Field
The invention belongs to the technical field of surface treatment of M50 steel; in particular to a Cr-Mo-Nb-W alloying method by M50 steel pulsed electron beam irradiation.
Background
As a novel technology, the irradiation of a large-area high-current pulse electron beam generates electron beam pulses with extremely high energy density through an electron gun to bombard the surface of a material, so that the surface of the material is instantaneously melted and solidified at the instantaneous high temperature generated by the electron beam to obtain a fine tissue or an unbalanced phase on the surface, and the change of the surface performance of the material is realized. An alloying layer is deposited on the surface of the substrate by magnetron sputtering, and then the alloying layer and the substrate can be melted and solidified simultaneously by electron beam irradiation, so that alloying is realized. The obtained alloying layer and the substrate are metallurgically bonded, so that the problem of weak bonding force between the coating prepared by other methods and the substrate is thoroughly solved. In addition, because the irradiation energy of the electron beam is concentrated and the time is extremely short, only a few materials close to the surface layer are melted, and most of the base material is still at room temperature, so the method does not change the roughness of the surface of the material. The method is particularly suitable for optimizing the surface property of precision materials such as bearings.
M50 steel is a common bearing steel and is often used in high temperature friction conditions such as aircraft engine bearings, turbine bearings, and the like. Under the working conditions, the better bearing needs high-temperature mechanical property and good stability, particularly needs a small friction coefficient at high temperature, particularly needs to consider the condition that the lubricating oil is interrupted, the friction coefficient between the bearing and the bearing bush needs to be small, and the condition that the temperature is increased due to the increase of the friction coefficient and the friction coefficient is increased due to the increase of the temperature is avoided.
Disclosure of Invention
Aiming at the problem of high-temperature friction and wear resistance of M50 steel, the invention provides that the Nb-W-Cr-Mo alloying treatment is carried out on the surface of M50 steel by combining the magnetron sputtering process with the high-current pulsed electron beam irradiation process, so that the high-temperature friction coefficient of the M50 steel is reduced, and the high-temperature friction and wear resistance is improved.
The invention discloses an Nb-W-Cr-Mo alloying method by M50 steel pulsed electron beam irradiation, which is carried out according to the following steps:
firstly, pretreating the surface of an M50 steel workpiece;
secondly, placing the workpiece on a workbench in a vacuum chamber, facing the surface to be processed of the workpiece to the electron gun, and vacuumizing to 4 × 10-4Pa~7×10-4Pa;
Step three, continuously introducing argon into the vacuum chamber, and then irradiating for 50-100 times under the conditions that the air pressure is 0.04-0.08 Pa and the accelerating voltage is controlled at 30 kv;
step four, performing magnetron sputtering on the surface to be treated of the workpiece by using a Mo target, a Cr target, a W target and a Nb target in sequence;
fifthly, turning the surface to be processed of the workpiece to face the electron beam, introducing argon into the vacuum chamber, and irradiating for 50-100 times under the conditions that the air pressure is 0.04-0.06 Pa and the accelerating voltage is controlled at 27 kv;
and step six, cooling for 20 +/-2 min, taking out and cooling in air to finish the process.
The method is further limited on the basis of the scheme, in the step one, the pretreatment is that grinding and polishing are carried out firstly, and then acetone and absolute ethyl alcohol are sequentially used for ultrasonic cleaning; wherein, the grinding and polishing are carried out by using sand paper of 320#, 600#, 800#, 1000#, 1500# and 2000# for gradual grinding, and a diamond polishing agent is used for polishing a sample to the surface roughness RaLess than or equal to 0.1 mu m. The ultrasonic cleaning time is 5 min-10 min.
Further, the magnetron sputtering of Mo target in the fourth step is carried out by the steps of vacuumizing to 6 × 10- 4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 143mA, the working voltage is 350v and the gas filling amount is 450sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, turning off the power supply, and cooling for 10min to 20 min.
Further, the magnetron sputtering of the Cr target in the fourth step is carried out by vacuumizing to 6 × 10- 4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 125mA, the working voltage is 400v and the gas filling amount is 600sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, turning off the power supply, and cooling for 10min to 20 min.
Further defined, in the fourth step, the magnetron sputtering of the W target is carried out by the steps of vacuumizing to 6 × 10- 4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 131mA, the working voltage is 380v and the gas filling amount is 505sccm, and depositing 1.5miAnd n, stopping introducing argon, stopping magnetron sputtering after 25min, turning off a power supply, and cooling for 10 min-20 min.
Further defining, in step four, the magnetron sputtering of Nb target is carried out by the steps of evacuating to 6 × 10- 4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 161mA, the working voltage is 310v and the gas filling amount is 580sccm, depositing for 20.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, turning off the power supply, and cooling for 10 min-20 min.
According to the invention, Nb, W, Cr and Mo are added into steel as alloy elements to prepare the Nb-W-Cr-Mo alloying coating, so that a combined effect is generated, and as the Nb-W-Cr-Mo is added, a magnelli phase oxide can be formed in a high-temperature friction process, the layered characteristic coating has a lower friction coefficient and has adhesive force with an M50 steel matrix, so that the high-temperature friction and wear properties of the M50 steel can be obviously improved.
Drawings
FIG. 1 is a cross-sectional view of a Nb-W-Cr-Mo alloyed layer on the surface of a high current pulsed electron beam;
FIG. 2 is a line scan of a surface Nb-W-Cr-Mo alloyed layer with a high current pulsed electron beam;
FIG. 3 is a surface topography of a Nb-W-Cr-Mo alloyed layer on a surface of a high current pulsed electron beam;
fig. 4 is a friction coefficient curve.
Detailed Description
Example 1: in the embodiment, the Nb-W-Cr-Mo alloying method by the pulse electron beam irradiation of the M50 steel is carried out according to the following steps:
grinding and polishing the surface of an M50 steel workpiece: firstly, sand paper of 320#, 600#, 800#, 1000#, 1500# and 2000# is adopted for gradual grinding, and a diamond polishing agent is used for polishing a sample to the surface roughness RaLess than or equal to 0.1 μm, respectively cleaning in acetone and anhydrous ethanol for 10min with ultrasonic cleaning instrument, and blow-drying with blower;
secondly, the workpiece is placed on a workbench in a vacuum chamber, the surface to be processed of the workpiece faces to the electron gun, and thenVacuum pumping is carried out to 6 × 10-4Pa;
Step three, continuously introducing argon into the vacuum chamber, and then irradiating for 50 times under the conditions that the air pressure is 0.06Pa and the accelerating voltage is controlled at 30 kv;
fourthly, performing magnetron sputtering on the surface to be processed of the workpiece by using a Mo target material, a Cr target material, a W target material and a Nb target in sequence, wherein the specific operation is realized by the following steps:
step 4.1, turning the surface to be processed of the workpiece to a Mo target (with the mass purity of 99.9 wt.%) and vacuumizing to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 143mA, the working voltage is 350v and the gas filling amount is 450sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, closing the power supply, and cooling for 10min (pink glow);
step 4.2, the surface to be processed of the workpiece is turned to a Cr target material (the mass purity is 99.9 wt.%) and vacuum pumping is carried out to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 125mA, the working voltage is 400v and the gas filling amount is 600sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, closing the power supply and cooling for 10min (blue glow);
4.3, turning the surface to be processed of the workpiece to a W target (the mass purity is 99.9 wt.%), and vacuumizing to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 131mA, the working voltage is 380v and the gas filling amount is 505sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, closing the power supply, and cooling for 10min (pink glow);
step 4.4, the surface to be processed of the workpiece is turned to an Nb target material (the mass purity is 99.9 wt.%), and the workpiece is vacuumized to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 161mA, the working voltage is 310v and the gas filling amount is 580sccm, depositing for 20.5min, and stopping introducing the argonStopping magnetron sputtering after 25min, turning off the power supply, and cooling for 10min (pink glow);
fifthly, turning the surface to be processed of the workpiece to face the electron beam, introducing argon into the vacuum chamber, and irradiating for 50 times under the conditions that the air pressure is 0.06Pa and the accelerating voltage is controlled at 22 kv;
and step six, cooling for 20min, taking out, and cooling in air to finish.
The cross-sectional morphology of the Nb-W-Cr-Mo alloyed layer on the surface of the high-current pulsed electron beam is shown in FIG. 1, the line scanning is shown in FIG. 2, and it can be seen from FIG. 1 and FIG. 2 that the content of Nb-W-Cr-Mo elements on the surface is obviously higher than that in the matrix after the deposition and alloying treatment, which indicates that the elements are enriched on the surface.
The surface morphology of the Nb-W-Cr-Mo alloyed layer on the surface of the high-current pulsed electron beam is shown in FIG. 3, and the result shows that the alloyed surface is basically flat and shallow pits exist.
It can be seen from FIG. 4 that the Nb-W-Cr-Mo alloyed coating prepared in example 1 has a significantly reduced coefficient of friction, and that the addition of Nb-W-Cr-Mo leads to the formation of oxides of the magnelli phase during high-temperature friction, which oxides have a lower coefficient of friction on the one hand and increase the adhesion of the oxide film to the M50 steel substrate on the other hand.
Claims (8)
1. An alloying method of M50 steel by Nb-W-Cr-Mo through pulsed electron beam irradiation, which is characterized in that the preparation method is carried out according to the following steps:
firstly, pretreating the surface of an M50 steel workpiece;
secondly, placing the workpiece on a workbench in a vacuum chamber, facing the surface to be processed of the workpiece to the electron gun, and vacuumizing to 4 × 10-4Pa~7×10-4Pa;
Step three, continuously introducing argon into the vacuum chamber, and then irradiating for 50-100 times under the conditions that the air pressure is 0.04-0.08 Pa and the accelerating voltage is controlled at 30 kv;
step four, performing magnetron sputtering on the surface to be treated of the workpiece by using a Mo target, a Cr target, a W target and a Nb target in sequence;
fifthly, turning the surface to be processed of the workpiece to face the electron beam, introducing argon into the vacuum chamber, and irradiating for 50-100 times under the conditions that the air pressure is 0.04-0.06 Pa and the accelerating voltage is controlled at 27 kv;
and step six, cooling for 20 +/-2 min, taking out and cooling in air to finish the process.
2. The method for alloying Nb-W-Cr-Mo by irradiating M50 steel with pulsed electron beam according to claim 1, wherein the pretreatment in the first step is grinding and polishing, and then ultrasonic cleaning with acetone and absolute ethyl alcohol in sequence.
3. The method for alloying Nb-W-Cr-Mo by irradiating M50 steel with pulsed electron beam as claimed in claim 2, wherein the polishing step comprises polishing the steel sample with 320#, 600#, 800#, 1000#, 1500# and 2000# sandpaper, and polishing the sample with diamond polishing agent to obtain surface roughness Ra≤0.1μm。
4. The alloying method of Nb-W-Cr-Mo by the pulsed electron beam irradiation of M50 steel as claimed in claim 2, wherein the ultrasonic cleaning time is 5-10 min.
5. The method for alloying M50 steel by irradiating Nb-W-Cr-Mo through pulsed electron beam according to claim 1, wherein the Mo target magnetron sputtering in the fourth step is performed by the steps of vacuumizing to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 143mA, the working voltage is 350v and the gas filling amount is 450sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, turning off the power supply, and cooling for 10min to 20 min.
6. The method for alloying M50 steel by irradiating Nb-W-Cr-Mo through pulsed electron beam according to claim 1, wherein the magnetron sputtering of Cr target in the fourth step is performed by vacuumizing to 6 × 10-4Pa, after the vacuum pumping is finished, the vacuum chamber is filled with the mixtureContinuously introducing argon gas, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 125mA, the working voltage is 400v and the gas charging amount is 600sccm, depositing for 1.5min, stopping introducing the argon gas, stopping the magnetron sputtering after 25min, turning off a power supply, and cooling for 10-20 min.
7. The method for alloying M50 steel by irradiating Nb-W-Cr-Mo through the pulsed electron beam according to claim 1, wherein the magnetron sputtering of the W target in the fourth step is performed by vacuumizing to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 131mA, the working voltage is 380v and the gas charging amount is 505sccm, depositing for 1.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, turning off the power supply, and cooling for 10 min-20 min.
8. The method of claim 1 in which the Nb-W-Cr-Mo alloying process by pulsed electron beam irradiation of M50 steel is performed by magnetron sputtering of Nb target in step four, wherein the step four is performed by vacuum pumping to 6 × 10-4Pa, after the vacuum pumping is finished, continuously introducing argon into the vacuum chamber, carrying out magnetron sputtering under the conditions that the working power is 50w, the working current is 161mA, the working voltage is 310v and the gas filling amount is 580sccm, depositing for 20.5min, stopping introducing the argon, stopping the magnetron sputtering after 25min, turning off the power supply, and cooling for 10 min-20 min.
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