Disclosure of Invention
The technology of the invention carries out arc light enhanced argon ion bombardment in vacuum coating equipment, designs a special structural layout, adopts arc ion plating as an ionization source, can provide high current density, simultaneously converts a columnar coating cathode opposite to the arc ion plating cathode into an anode in the process, guides high-density electron current to pass through a cleaned workpiece area, and ensures that each angle of the workpiece obtains Ar+The flow is sufficiently cleaned to ensure that it is carried out at a lower bias, thereby preventing excessive damage to the workpiece by bombardment.
The technical means adopted by the invention are as follows:
a vacuum coating device comprises a device body, a vacuum cavity, an electric arc enhancing source, a cylindrical magnetron sputtering target position, a baffle and a material tray, wherein the electric arc enhancing source, the cylindrical magnetron sputtering target position, the baffle and the material tray are arranged in the vacuum cavity; the cylindrical magnetron sputtering target positions are positioned at four vertex angles of the vacuum chamber, wherein an electric arc enhancing source is arranged between the two cylindrical magnetron sputtering target positions, and a baffle is arranged in front of the electric arc enhancing source;
the vacuum coating equipment comprises a magnetron sputtering mode and a cleaning mode, when the cleaning mode is adopted, two cylindrical magnetron sputtering target positions on the opposite side of the arc enhancement source can be used as arc enhancement target positions, and the arc enhancement target positions are anode target positions.
A novel ion cleaning process based on a hard alloy surface ta-C film is characterized by comprising the following steps of:
(1) cleaning impurities on the surface of the plasma matrix by ultrasonic waves, and then loading the plasma matrix into vacuum coating equipment;
(2) arc light enhanced argon ion bombardment is carried out in vacuum coating equipment to remove impurities on the surface of a substrate, and the working steps are as follows:
s1: vacuumizing and heating a vacuum cavity of the vacuum coating equipment;
s2: starting a circular arc enhancing source, using Ti as a target source, and generating a large amount of Ti ions after starting+And an electron e-Titanium ion Ti+A baffle plate splashed in front of the target prevents the pollution of a workpiece to be cleaned on the material tray;
s3: when S2 is carried out, argon Ar is introduced into the vacuum cavity, two arc enhancement target positions on the opposite side of the circular arc enhancement source are connected with the positive electrode of the power supply, the columnar coating cathode is converted into an anode in the process, and electrons generated by S2 are guided to and pass through the workpiece area to be cleaned;
s4: a large number of electrons e generated-Bypassing the baffle plate, attracting by the arc-enhanced target position with positive potential on the opposite side, and colliding with the argon atoms entering the vacuum chamber to form high-density Ar+、Ar++A stream;
s5: biasing the material tray negatively, generating a large amount of argon ions Ar in S4+、Ar++Bombarding a workpiece to be cleaned on the material tray under the action of an electric field, and cleaning impurities on the surface of the workpiece;
s6: after cleaning, switching two arc enhanced target positions connected with the anode to a cathode to be used as a coating source of the next step, rotating 180 degrees at the same time, introducing argon Ar, cleaning the target surface by self-sputtering in a magnetron sputtering mode, sputtering impurities on the surface of the target surface onto the wall of the vacuum chamber, and arranging no baffle plate in front of the target;
(3) entering the vacuum coating process step.
Further, the frequency of the ultrasonic wave in the step (1) is 25-45 kHz.
Further, in the step (2), in S1, the temperature of the vacuum chamber is heated to 350-550 ℃, the moisture on the surface of the substrate is removed, and the vacuum degree reaches 6 multiplied by 10-3Pa or less.
Further, in the step (2), the argon Ar flow in S3 is 40-160 sccm, and the two arc strengthening target positions are connected with the power positive electrode by 40-200V.
Further, in the step (2), aiming at the S5, the negative bias voltage of the material tray is 120-300V, the cleaning time is 15-40 min, and a large amount of argon ions Ar generated in the S4+、Ar++The workpiece to be cleaned on the material tray is bombarded under the action of the electric field, so that the workpiece can be prevented from being damaged due to the excessive bombardment effect of the overhigh metal ion flow on the precise workpiece under the condition of using lower bias voltage.
Further, in the step (2), the flow rate of Ar gas in S6 is 50-200 sccm.
Compared with the prior art, the invention has the following advantages:
by adopting the technical scheme of the invention, the workpiece can be prevented from being excessively damaged by ion bombardment generated by high bias voltage, the electron flow with higher density can be kept, the high-density electron flow is guided to the area of the cleaned workpiece through the conversion of the cathode and the anode, the full cleaning of each angle can be ensured, and the film-substrate binding force can be better improved. The method has the advantages of reducing the damage to the workpiece, fully cleaning, improving the production efficiency, promoting better film-substrate binding force, improving the deposition thickness and hardness of the film and the like, and can be applied to the pretreatment process of the hard alloy plated with the ta-C film.
Detailed Description
The technical solution of the present invention will be further described with reference to the accompanying drawings and specific examples, but the present invention is not limited to the following examples, which are conventional processes unless otherwise specified, and the starting materials are commercially available from the public unless otherwise specified.
The cleaning process of the invention uses the following instruments:
(1) m308457 ultrasonic cleaner.
The test method adopted by the invention comprises the following steps:
(1) quanta FEG field emission environment scanning electron microscope (with spectrometer);
(2) measuring hardness and elastic modulus by a NANO Indenter G200 type NANO Indenter;
(3) WS-2005 coating scratch tester
(4) The ESCALB 250 model atomic force microscope was used to observe the surface roughness.
The process comprises the following steps:
(1) cleaning impurities on the surface of the plasma matrix by ultrasonic waves, and then loading the plasma matrix into vacuum coating equipment;
(2) performing arc light enhanced argon ion bombardment in vacuum coating equipment to remove impurities on the surface of the substrate;
the equipment body comprises a vacuum cavity, and an electric arc enhancing source, a cylindrical magnetron sputtering target position, a baffle and a material tray which are arranged in the vacuum cavity; the cylindrical magnetron sputtering target positions are positioned at four vertex angles of the vacuum chamber, wherein an electric arc enhancing source is arranged between the two cylindrical magnetron sputtering target positions, and a baffle is arranged in front of the electric arc enhancing source; the device comprises a magnetron sputtering mode and a cleaning mode, when the cleaning mode is adopted, two cylindrical magnetron sputtering target positions on the opposite side of the arc enhancement source can be used as arc enhancement target positions, and the arc enhancement target positions are anode target positions at the moment, as shown in the attached figure 1;
the specific working steps are as follows:
s1: vacuumizing a vacuum cavity of vacuum coating equipment, heating to 350-550 ℃, and enabling the vacuum degree to reach 6 multiplied by 10-3Pa below;
s2: starting the circulararc enhancing source 1, using Ti as a target source, and generating a large amount of Ti ions after starting+And an electron e-Titanium ions are sprayed on thefront baffle 3 of the target to prevent polluting workpieces to be cleaned on thematerial tray 4;
s3: while S2 is carried out, argon Ar is introduced into the vacuum cavity, the flow rate is 40-160 sccm, two arcenhancement target positions 2 on the opposite side of the circular arc enhancement source are connected with a power supply anode by 40-200V, and electrons generated by S2 are guided to and pass through a workpiece area to be cleaned;
s4: a large number of electrons e generated-Bypassing the baffle plate, being attracted by the opposite side positive potential arc strengtheningtarget position 2, colliding with argon atoms entering the vacuum chamber to form high-density Ar+、Ar++A stream;
s5: the material tray is negatively biased to 120-300V; a large amount of Ar ion generated in S4+、Ar++Bombarding a workpiece to be cleaned on thematerial tray 4 under the action of an electric field, and cleaning impurities on the surface of the workpiece; the cleaning duration is 15-40 min;
s6: after cleaning, switching the two circular arc enhancedtarget positions 2 connected with the anode to the cathode to be used as a film coating source in the next step, simultaneously rotating 180 ℃, introducing argon Ar with the flow of 50-200 sccm, cleaning the target surface by self-sputtering in a magnetron sputtering mode, and sputtering impurities on the surface of the target onto the wall of the vacuum chamber without arranging a baffle in front of the target;
(3) entering the vacuum coating process step.
Example 1
(1) Cleaning impurities on the surface of the plasma hard alloy substrate by ultrasonic waves at 30kHz, and charging;
(2) carrying out arc light enhanced argon ion bombardment in vacuum coating equipment to remove impurities on the surface of the hard alloy substrate;
(3) the vacuum cavity of the vacuum coating equipment is vacuumized, and the vacuum degree reaches 1.5 multiplied by 10-3Pa, and heating to 450 ℃;
(4) starting the circulararc enhancing source 1, using Ti as a target source, and generating a large amount of Ti ions after starting+And an electron e-Titanium ions are sprayed on thefront baffle 3 of the target to prevent polluting workpieces to be ion-cleaned on thematerial tray 4;
(5) meanwhile, the circular arc enhanced source connects two arcenhanced target positions 2 on the side with the power supply anode of 150V, and a large amount of generated electrons are attracted;
(6) simultaneously introducing argon Ar into the vacuum cavity with the flow of 85 sccm;
(7) a large number of electrons e generated-Bypassing the baffle plate, being attracted by the opposite side positive potential arc strengtheningtarget position 2, colliding with argon atoms entering the vacuum chamber to form high-density Ar+、Ar++A stream;
(8) thematerial tray 4 is negatively biased to 200V; a large amount of Ar ions generated in step (7)+Bombarding a workpiece to be cleaned on thematerial tray 4 under the action of an electric field, and cleaning impurities on the surface of the workpiece for 30 min;
(9) after cleaning, switching the two arcenhancement target positions 2 connected with the anode to the cathode to be used as a coating source of the next step, rotating 180 degrees at the same time, introducing argon Ar with the flow of 110sccm, cleaning the target surface by sputtering in a magnetron sputtering mode, and sputtering impurities on the surface of the target surface onto the wall of the vacuum chamber;
(10) and entering a vacuum coating process step to obtain the ta-C film with excellent performance, namely the roughness of the ta-C coating Ra0.08 mu m, the hardness of the coating 46.3GPa, the film-substrate binding force reaching 57N and the coating thickness being 0.55 mu m.
Example 2
(1) Cleaning impurities on the surface of the plasma hard alloy substrate by ultrasonic waves at 40kHz, and charging;
(2) carrying out arc light enhanced argon ion bombardment in vacuum coating equipment to remove impurities on the surface of the hard alloy substrate;
(3) the vacuum cavity of the vacuum coating equipment is vacuumized, and the vacuum degree reaches 4.5 multiplied by 10-3Pa, and heating to 370 ℃;
(4) starting the circulararc enhancing source 1, using Ti as a target source, and generating a large amount of Ti ions after starting+And an electron e-Titanium ions are sprayed on thefront baffle 3 of the target to prevent polluting workpieces to be cleaned on thematerial tray 4;
(5) meanwhile, the circular arc reinforcing source is connected with the two arc reinforcingtarget positions 2 at the side by a power supply anode 80V, and a large amount of generated electrons are attracted;
(6) simultaneously introducing argon Ar into the vacuum cavity with the flow rate of 112 sccm;
(7) a large number of electrons e generated-Bypassing the baffle plate, being attracted by the opposite side positive potential arc strengtheningtarget position 2, colliding with argon atoms entering the vacuum chamber to form high-density Ar+,Ar++A stream;
(8) the material tray is connected with a negative bias voltage of 260V of 4; a large amount of Ar ions generated in step (7)+Bombarding a workpiece to be cleaned on thematerial tray 4 under the action of an electric field, and cleaning impurities on the surface of the workpiece; the cleaning duration is 25 min;
(9) after cleaning, switching the two arcenhanced target positions 2 connected with the anode to the cathode to be used as a film coating source in the next step, simultaneously rotating 180 ℃, introducing argon Ar with the flow of 170sccm, cleaning the target surface by sputtering in a magnetron sputtering mode, and sputtering impurities on the surface of the target surface onto the wall of the vacuum chamber;
(10) and entering a vacuum coating process step to obtain the ta-C film with excellent performance, namely the roughness of the ta-C coating Ra0.09 mu m, the hardness of the coating 31.5GPa, the film-substrate binding force of 51N and the coating thickness of 0.32 mu m.
Example 3
(1) Cleaning impurities on the surface of the plasma hard alloy substrate by ultrasonic waves at 40kHz, and charging;
(2) carrying out arc light enhanced argon ion bombardment in vacuum coating equipment to remove impurities on the surface of the hard alloy substrate;
(3) the vacuum cavity of the vacuum coating equipment is vacuumized, and the vacuum degree reaches 4.5 multiplied by 10-3Pa, and heating to 550 ℃;
(4) starting the circulararc enhancing source 1, using Ti as a target source, and generating a large amount of Ti ions after starting+And an electron e-Titanium ions are sprayed on thefront baffle 3 of the target to prevent polluting workpieces to be cleaned on thematerial tray 4;
(5) meanwhile, the circular arc reinforcing source is connected with two arc reinforcingtarget positions 2 at the side through a power supply anode 40V, and a large amount of generated electrons are attracted;
(6) simultaneously introducing argon Ar into the vacuum cavity with the flow rate of 160 sccm;
(7) a large number of electrons e generated-Bypassing the baffle plate, being attracted by the opposite side positive potential arc strengtheningtarget position 2, colliding with argon atoms entering the vacuum chamber to form high-density Ar+,Ar++A stream;
(8) thematerial tray 4 is negatively biased to 160V; a large amount of Ar ions generated in step (7)+Bombarding a workpiece to be cleaned on thematerial tray 4 under the action of an electric field, and cleaning impurities on the surface of the workpiece; cleaning for 40 min;
(9) after cleaning, switching the two arcenhanced target positions 2 connected with the anode to the cathode to be used as a film coating source in the next step, simultaneously rotating 180 ℃, introducing argon Ar with the flow of 170sccm, cleaning the target surface by sputtering in a magnetron sputtering mode, and sputtering impurities on the surface of the target surface onto the wall of the vacuum chamber;
(10) and entering a vacuum coating process step to obtain the ta-C film with excellent performance, namely the roughness of the ta-C coating Ra0.09 mu m, the hardness of the coating 28.5GPa, the film-substrate binding force of 53N and the coating thickness of 0.45 mu m.
Example 4
(1) Cleaning impurities on the surface of the plasma hard alloy substrate by ultrasonic waves at 30kHz, and charging;
(2) carrying out arc light enhanced argon ion bombardment in vacuum coating equipment to remove impurities on the surface of the hard alloy substrate;
(3) the vacuum cavity of the vacuum coating equipment is vacuumized, and the vacuum degree reaches 5.0 multiplied by 10-3Pa, and heating to 350℃;
(4) Starting the circulararc enhancing source 1, using Ti as a target source, and generating a large amount of Ti ions after starting+And an electron e-Titanium ions are sprayed on thefront baffle 3 of the target to prevent polluting workpieces to be cleaned on thematerial tray 4;
(5) meanwhile, the circular arc enhanced source connects the two arcenhanced target positions 2 on the side with the positive electrode of the power supply of 200V, and a large amount of generated electrons are attracted;
(6) simultaneously introducing argon Ar into the vacuum cavity with the flow rate of 40 sccm;
(7) a large number of electrons e generated-Bypassing the baffle plate, being attracted by the opposite side positive potential arc strengtheningtarget position 2, colliding with argon atoms entering the vacuum chamber to form high-density Ar+,Ar++A stream;
(8) thematerial tray 4 is negatively biased to 300V; a large amount of Ar ions generated in step (7)+Bombarding a workpiece to be cleaned on thematerial tray 4 under the action of an electric field, and cleaning impurities on the surface of the workpiece; the cleaning duration is 25 min;
(9) after cleaning, switching the two arcenhanced target positions 2 connected with the anode to the cathode to be used as a film coating source in the next step, simultaneously rotating 180 ℃, introducing argon Ar with the flow of 170sccm, cleaning the target surface by sputtering in a magnetron sputtering mode, and sputtering impurities on the surface of the target surface onto the wall of the vacuum chamber;
(10) and entering a vacuum coating process step to obtain the ta-C film with excellent performance, namely the roughness of the ta-C coating Ra0.09 mu m, the hardness of the coating 33.5GPa, the film-substrate binding force of 48N and the coating thickness of 0.6 mu m.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.